CN116219530A - Crystal carrier and methyl amine bromine lead perovskite single crystal growth method - Google Patents
Crystal carrier and methyl amine bromine lead perovskite single crystal growth method Download PDFInfo
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- CN116219530A CN116219530A CN202310081355.7A CN202310081355A CN116219530A CN 116219530 A CN116219530 A CN 116219530A CN 202310081355 A CN202310081355 A CN 202310081355A CN 116219530 A CN116219530 A CN 116219530A
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- crystal
- baffle
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- growth
- single crystal
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- 239000013078 crystal Substances 0.000 title claims abstract description 123
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 title description 6
- XQMUOIMHJMRRGK-UHFFFAOYSA-M bromolead Chemical compound [Pb]Br XQMUOIMHJMRRGK-UHFFFAOYSA-M 0.000 title description 3
- 238000002109 crystal growth method Methods 0.000 title description 2
- 238000000034 method Methods 0.000 claims abstract description 26
- VLSWWRJVKAPDDQ-UHFFFAOYSA-N [Pb].[Br].CN Chemical compound [Pb].[Br].CN VLSWWRJVKAPDDQ-UHFFFAOYSA-N 0.000 claims abstract description 17
- 238000003756 stirring Methods 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 10
- 238000004781 supercooling Methods 0.000 claims description 6
- ISWNAMNOYHCTSB-UHFFFAOYSA-N methanamine;hydrobromide Chemical compound [Br-].[NH3+]C ISWNAMNOYHCTSB-UHFFFAOYSA-N 0.000 claims description 5
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- MJFXORGVTOGORM-UHFFFAOYSA-L lead(2+) methanamine dibromide Chemical compound [Pb+2].[Br-].CN.[Br-] MJFXORGVTOGORM-UHFFFAOYSA-L 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 13
- 230000000694 effects Effects 0.000 description 3
- -1 Methylamine bromolead Chemical compound 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000012296 anti-solvent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000005669 field effect Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/54—Organic compounds
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
The invention discloses a crystal carrying frame and a method for growing a methylamine bromine lead perovskite single crystal, which belong to the technical field of crystal growth. According to the crystal carrier and the method for growing the methylamine bromine lead perovskite single crystal, provided by the invention, a transverse drum-type rotation mode is adopted, so that the lower layer of the solution can be fully stirred, the uniformity of the whole solute is ensured, and the problem of white streak and other defects in the crystal growth process can be effectively solved.
Description
Technical Field
The invention relates to a crystal carrier and a method for growing a methylamine bromine lead perovskite single crystal, belonging to the technical field of crystal growth.
Background
Methylamine bromolead (CH) 3 NH 3 PbBr 3 ) Perovskite crystalThe material has the advantages of large carrier diffusion length, high carrier mobility, low defect density, high light absorption coefficient and the like, and has great potential in various fields such as solar cells, light-emitting diodes, field effect transistors, photodetectors, memristors, lasers and the like.
Common growth modes of the methylamine bromine lead perovskite single crystal include an evaporation method, a cooling method, an antisolvent diffusion method, a reverse-temperature crystallization method and the like, solute in a crystal growth solution is not uniformly distributed due to gravity, the solute is difficult to ensure uniform distribution of the upper layer and the lower layer in the solution in the rotating process of a crystal carrying frame, so that macroscopic defects such as white lines and the like appear in the crystal growth process, once the defects are generated, crystals at the defect positions grow rapidly, so that the growth of main crystals is stopped, the expected size cannot be reached, and the growth of the crystals fails.
Therefore, the invention provides a crystal carrier and a method for growing a methylamine bromine lead perovskite single crystal.
Disclosure of Invention
The invention provides a crystal carrier and a method for growing a methylamine bromine lead perovskite single crystal, which adopts a transverse drum type rotation mode, can fully stir the lower layer of a solution, ensures the uniformity of the whole solute, can effectively solve the problem of white lines and other defects in the crystal growth process, and is beneficial to growing the high-quality and large-size methylamine bromine lead perovskite single crystal.
In a first aspect, the present invention provides a carrier. The crystal carrying frame can fully stir the lower layer of the solution in a drum-type stirring rotation mode of the transverse rotating shaft, and the uniformity of solute is ensured.
The utility model provides a crystal carrying frame, includes first baffle, second baffle and connects the backup pad of first baffle and second baffle, wherein, be connected with the connecting rod that is used for connecting the actuating source on first baffle and/or the second baffle, the connecting rod makes the actuating source drive the crystal carrying frame is drum-type rotary motion, and this crystal carrying frame is with the drum-type stirring rotation mode of horizontal rotation axis.
Optionally, the opposite sides of the first baffle and the second baffle are provided with a hole channel for embedding the end part of the seed crystal, so that the seed crystal is conveniently fixed between the first baffle and the second baffle, and the hole channel can be cuboid or can be in other shapes suitable for extending into the end part of the seed crystal.
Optionally, the first baffle and/or the second baffle are/is provided with a fixing nut for locking the end part of the seed crystal, and the seed crystal can be better fixed by locking the end part of the seed crystal through rotating the fixing nut, so that the stability of the seed crystal is kept.
Optionally, be provided with the interference flow face in the backup pad, the backup pad both plays the frame effect of supporting whole crystal-carrying frame, can play the stirring effect again when the crystal-carrying frame rotates, has further guaranteed the homogeneity of solute.
Optionally, the cross section of the support plate is arranged in a triangle shape, so that the outer side surface of the support plate forms a turbulent flow surface.
Optionally, a stirring paddle is connected to the first baffle and/or the second baffle for stirring the crystal growth solution.
Optionally, the stirring paddle is disposed on an outer side surface of the first baffle plate and/or the second baffle plate.
In a second aspect, the invention provides a method for growing a methylamine bromine lead perovskite single crystal, which is prepared by using the crystal carrier according to any one of the first aspects, and comprises the following steps:
fixing seed crystals between the first baffle plate and the second baffle plate;
placing the crystal carrier in a growth tank loaded with a growth solution;
the driving source is started to drive the crystal carrying frame to do drum-type rotary motion.
Alternatively, the growth solution is obtained by dissolving methyl ammonium bromide and lead bromide in N, N-dimethylformamide.
Alternatively, the saturation point temperature of the growth solution is 25-35 ℃.
Alternatively, the growth solution is drawn into the growth tank through a 0.1 μm filter cartridge.
Optionally, when the crystal carrier is placed in the growth tank loaded with the growth solution, the temperature of the growth tank is adjusted to 15-25 ℃, and the crystal growth solution is subjected to supercooling treatment.
Alternatively, the supercooling treatment time is 24 to 48 hours.
Optionally, after supercooling the crystal growth solution, adjusting the temperature of the growth tank to 2-5 ℃ below the saturation point temperature, dissolving the seed crystal, and raising the temperature of the growth tank to 3-5 ℃ above the saturation point temperature when the slightly soluble surface of the seed crystal is smooth.
Optionally, the rotation speed of the crystal carrying frame is 30-60r/min when the crystal carrying frame rotates in a drum type, the rotation speed of the crystal carrying frame can be adjusted at any time according to the growth state of crystals, the stirring of the growth solution can be accelerated by increasing the rotation speed, and the crystal carrying frame is suitable for the state of higher crystal growth speed, and the defect of crystals due to the excessively high growth speed can be avoided under the rotation speed range.
Optionally, when the driving source is started to drive the crystal carrier to perform drum-type rotary motion, the temperature of the growth tank is increased at a heating rate of 0.1-1 ℃/d.
The invention has the beneficial effects that:
1) According to the crystal carrier and the method for growing the methylamine bromine lead perovskite single crystal, provided by the invention, a transverse drum-type rotation mode is adopted, so that the lower layer of the solution can be fully stirred, the uniformity of the whole solute is ensured, and the problem of white streak and other defects in the crystal growth process can be effectively solved;
2) Meanwhile, in the traditional rotation mode, once the mixed crystal appears on the crystal carrier, the mixed crystal can be contacted with the main crystal body to cause the defect of the crystal, so that the crystal growth fails.
Drawings
FIG. 1 is a front view of a carrier in accordance with embodiment 1 of the present invention;
FIG. 2 is a left side view of the susceptor in embodiment 1 of the present invention;
FIG. 3 is a schematic representation of a single crystal of methylamine-bromolead perovskite according to example 2 of the invention.
List of parts and reference numerals:
1-a first baffle; 2-a second baffle; 3-supporting plates; 4-stirring paddles; 5-fixing the nut; 6-connecting rods; 7-seed crystal; 8-pore canal.
Detailed Description
The present invention is described in detail below with reference to examples, but the present invention is not limited to these examples.
Unless otherwise indicated, all starting materials in the examples of the present invention were purchased commercially.
Example 1
As shown in fig. 1-2, the present embodiment discloses a carrier for rapid growth of a single crystal of methylamine bromine lead perovskite, the carrier comprising a disk-shaped first baffle plate 1 and a disk-shaped second baffle plate 2; two support plates 3; four rectangular stirring paddles 4; a fixing nut 5; a connecting rod 6; rectangular duct 8. The support plate 3 is connected with the first baffle plate 1 and the second baffle plate 3 to play a role of supporting, and the section of the support plate 3 in the embodiment is triangular to form a disturbing flow surface, and the stirring effect is also played when the support plate rotates; the first baffle plate 1 and the second baffle plate 2 are used for placing strip or sheet seed crystals 7, and the seed crystals 7 in the embodiment are arranged in a sheet shape; the stirring paddles 4 are sequentially distributed on the upper surface of the first baffle plate 1 and the lower surface of the second baffle plate 2 and are used for stirring the crystal growth solution; the connecting rod 6 is used for connecting a motor (driving source) and can drive the crystal carrier to rotate; the pore canal 8 is respectively positioned on the lower surface of the first baffle plate 1 and the upper surface of the second baffle plate 2 and is used for placing seed crystal 7; the fixed nut 5 is positioned at the center of the second baffle plate 2 and is used for keeping the seed crystal 7 stable. The crystal carrying frame in the embodiment is provided with a transverse rotating shaft, so that the flaky or strip-shaped seed crystal is transversely fixed in the middle of the crystal carrying frame, and a motor drives the crystal carrying frame to rotate in a transverse drum-type rotating mode, so that the lower layer of the solution is fully stirred, the uniformity of the whole solute is ensured, and the problems caused by white lines and other defects in the crystal growth process can be effectively solved.
Example 2
The embodiment discloses a method for growing a methylamine bromine lead perovskite single crystal, which specifically comprises the following steps:
(1) Methyl ammonium bromide (CH) as a growth material 3 NH 3 Br) and lead bromide (PbBr) 2 ) Dissolving in N, N-Dimethylformamide (DMF) to obtain a crystal growth solution, and measuring the saturation point of the crystal growth solution to be 30 ℃;
(2) Putting sheet seed crystals 7 into the holes 8 of the first baffle plate 1 and the second baffle plate 2, and rotating the fixing nuts 5 to fix the seed crystals 7;
(3) The temperature of the growth tank is adjusted to 20 ℃, and the crystal growth solution is supercooled for 10 hours;
(4) Pumping the growth solution into the growth tank through a 0.1 μm filter element;
(5) Adjusting the temperature of the growth tank to 27 ℃ to dissolve the seed crystal 7;
(6) When the seed crystal 7 is slightly dissolved and the surface is smooth, the temperature of the growth groove is increased to 35 ℃;
(7) The motor is started to enable the crystal carrying frame to rotate in a roller rotating mode, the rotating speed of the motor is 30r/min, and the motor drives the crystal carrying frame to rotate in a positive rotation-stop-reverse rotation mode;
(8) The temperature of the growth tank is raised at a heating rate of 0.5 ℃/d, so that the methylamine bromine lead perovskite single crystal can be grown, as shown in figure 3.
The crystal carrying frame and the method for growing the methyl amine bromine lead perovskite single crystal provided by the invention are used for solving the problem of uneven stirring caused by the rotation of a traditional horizontal clockwise (counterclockwise) needle, and rotating in a horizontal roller mode. Solute in the crystal growth solution must have uneven solute distribution due to gravity, and solute at the bottom of the solution is far greater than that at the top of the solution, so that the crystal growth is required to adopt a rotating mode, a common rotating needle rotates when water is adopted smoothly (in reverse time), and the crystal carrier is difficult to ensure even distribution of the solute in the upper layer and the lower layer of the solution in the rotating process, so that macroscopic defects such as white lines and the like appear in the crystal growth process. The rotary mode of the roller adopted by the invention can fully stir the lower layer of the solution, ensure the uniformity of the whole solute and effectively solve the defects of white lines and the like in the crystal growth process. Meanwhile, in the conventional rotation method, once the impurity crystal appears on the crystal carrier, the impurity crystal contacts with the main crystal body to cause the defect of the crystal, so that the crystal growth fails. According to the rotating mode, even if mixed crystals appear in the growth process, the mixed crystals can be rotated to the bottom of the growth groove, the growth of the main crystal is not affected, and the high-quality and large-size methylamine-bromine-lead perovskite single crystal can be grown, so that the method has the advantages of convenience in operation and low cost.
While the invention has been described in terms of preferred embodiments, it will be understood by those skilled in the art that various changes and modifications can be made without departing from the scope of the invention, and it is intended that the invention is not limited to the specific embodiments disclosed.
Claims (10)
1. The utility model provides a crystal carrying frame which characterized in that, includes first baffle, second baffle and connects the backup pad of first baffle and second baffle, wherein, be connected with the connecting rod that is used for connecting the actuating source on first baffle and/or the second baffle, the connecting rod makes the actuating source drive the crystal carrying frame makes drum-type rotary motion.
2. The carrier of claim 1, wherein the opposite sides of the first baffle and the second baffle are each provided with a hole for embedding a seed crystal end.
3. The carrier of claim 2, wherein a retaining nut is provided on the first baffle and/or the second baffle for locking the seed crystal end.
4. The carrier of claim 1, wherein the support plate is provided with a flow disrupting surface;
preferably, the cross section of the support plate is arranged in a triangle shape so that the outer side surface of the support plate forms a turbulent flow surface.
5. The carrier of claim 1, wherein the first baffle and/or the second baffle are/is connected with a stirring paddle;
preferably, the stirring paddles are arranged on the outer side surface of the first baffle plate and/or the second baffle plate.
6. A method for growing a single crystal of methylamine-bromine-lead perovskite, characterized in that it is prepared by using the carrier according to any one of claims 1 to 5, comprising the steps of:
fixing seed crystals between the first baffle plate and the second baffle plate;
placing the crystal carrier in a growth tank loaded with a growth solution;
the driving source is started to drive the crystal carrying frame to do drum-type rotary motion.
7. The method for growing a single crystal of methylamine lead bromide perovskite as claimed in claim 6, wherein the growth solution is obtained by dissolving methylammonium bromide and lead bromide in N, N-dimethylformamide;
preferably, the saturation point temperature of the growth solution is 25-35 ℃.
8. The method for growing a single crystal of methylamine-bromine-lead perovskite according to claim 7, wherein,
when the crystal carrying frame is placed in a growth tank loaded with growth solution, the temperature of the growth tank is adjusted to 15-25 ℃, and supercooling treatment is carried out on the crystal growth solution;
preferably, the supercooling treatment time is 24-48 hours;
preferably, after supercooling the crystal growth solution, adjusting the temperature of the growth tank to 2-5 ℃ below the saturation point temperature, dissolving the seed crystal, and raising the temperature of the growth tank to 3-5 ℃ above the saturation point temperature when the slightly soluble surface of the seed crystal is smooth.
9. The method for growing a single crystal of methylamine-bromine-lead perovskite according to claim 6 wherein the rotation speed of the carrier is 30-60r/min when the carrier is in drum-type rotation.
10. The method for growing a single crystal of methylamine-bromine-lead perovskite according to claim 6 wherein when the drive source is started to drive the crystal carriage to perform drum-type rotary motion, the temperature of the growth tank is raised at a heating rate of 0.1-1 ℃/d.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310081355.7A CN116219530A (en) | 2023-02-03 | 2023-02-03 | Crystal carrier and methyl amine bromine lead perovskite single crystal growth method |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310081355.7A CN116219530A (en) | 2023-02-03 | 2023-02-03 | Crystal carrier and methyl amine bromine lead perovskite single crystal growth method |
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| CN116219530A true CN116219530A (en) | 2023-06-06 |
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| CN1381618A (en) * | 2001-04-12 | 2002-11-27 | 三菱重工业株式会社 | Protein crystallization equipment and protein crystallization method |
| CN1798881A (en) * | 2003-03-17 | 2006-07-05 | 财团法人大阪产业振兴机构 | Method for producing group iii nitride single crystal and apparatus used therefor |
| WO2011034165A1 (en) * | 2009-09-18 | 2011-03-24 | 日本化学工業株式会社 | Continuous crystalizizer |
| CN105113004A (en) * | 2015-09-01 | 2015-12-02 | 北京大学东莞光电研究院 | Group-III nitride crystal growing device |
| CN105671640A (en) * | 2015-12-29 | 2016-06-15 | 东南大学 | Layered large-size hybridized perovskite microcrystal material and preparation method thereof |
-
2023
- 2023-02-03 CN CN202310081355.7A patent/CN116219530A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1381618A (en) * | 2001-04-12 | 2002-11-27 | 三菱重工业株式会社 | Protein crystallization equipment and protein crystallization method |
| CN1798881A (en) * | 2003-03-17 | 2006-07-05 | 财团法人大阪产业振兴机构 | Method for producing group iii nitride single crystal and apparatus used therefor |
| WO2011034165A1 (en) * | 2009-09-18 | 2011-03-24 | 日本化学工業株式会社 | Continuous crystalizizer |
| CN105113004A (en) * | 2015-09-01 | 2015-12-02 | 北京大学东莞光电研究院 | Group-III nitride crystal growing device |
| CN105671640A (en) * | 2015-12-29 | 2016-06-15 | 东南大学 | Layered large-size hybridized perovskite microcrystal material and preparation method thereof |
Non-Patent Citations (2)
| Title |
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| H•E•毕勒，D•维斯腾贝格: "《合理的防腐蚀设计》", vol. 1, 30 June 1990, 北京：化学工业出版社, pages: 60 * |
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