CN106637403B - A kind of preparation method of perovskite monocrystalline - Google Patents
A kind of preparation method of perovskite monocrystalline Download PDFInfo
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- CN106637403B CN106637403B CN201611066423.9A CN201611066423A CN106637403B CN 106637403 B CN106637403 B CN 106637403B CN 201611066423 A CN201611066423 A CN 201611066423A CN 106637403 B CN106637403 B CN 106637403B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- 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
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Abstract
The invention discloses a kind of preparation methods of perovskite monocrystalline, including taking the first halide and the second halide to mix, and with polar solvent stirring and dissolving, perovskite solution is made, the mass ratio of the first halide, the second halide and polar solvent requires to keep perovskite solution supersaturated;Perovskite solution is filtered processing;The perovskite solution for being filtered processing is placed in hydrophobic container, perovskite monocrystalline is precipitated in heating.Select hydrophobic material as the growing container of perovskite monocrystalline in the present invention, due to the hydrophobicity of hydrophobic chamber wall, the nucleus number generated on hydrophobic chamber wall is sharply reduced, the monocrystalline quantity grown is opposite to be reduced, the crystal grown in unit time is bigger, the quantity of broken grain is reduced, and solution utilization rate gets a promotion, and crystal quality significantly improves.
Description
Technical field
The invention belongs to photoelectric material and single crystal preparation fields, more particularly, to a kind of preparation side of perovskite monocrystalline
Method.
Background technique
In nearest several years, novel perovskite material shows pole in fields such as photovoltaic, luminous, laser, photodetections
Big application value becomes one of the hot spot of investigation of materials in the world.
When crystals particle three-dimensional space in it is regular, be periodically arranged, crystal is whole three in other words
Dimension is made of on direction the same space grid, and particle when being arranged as long-range order, can claim this crystalline substance in space in entire crystal
Body is monocrystalline.
Compared to the polycrystal film of perovskite, perovskite monocrystalline illustrates more preferably thermal stability, broader light absorption model
It encloses, lower hole concentration and higher carrier mobility.It is expected that using monocrystalline perovskite solar battery can be with
Obtain better photoelectric conversion efficiency;Simultaneously because perfection of crystal and less defect, single crystal device also have more preferably
Stability.
Currently, the preparation method of perovskite monocrystalline mainly includes anti-solvent method, cooling crystallization method, heating crystallization method, top
Seed crystal solution growth method, slow evaporation solvent method, Bridgman method etc., wherein heating crystallization method with equipment the simple, speed of growth
Fastly, the features such as operation is simple is widely used.2015, the team led by the Dalian Chemistry and Physics Institute, Chinese Academy of Sciences Liu Shengzhong researcher
Normal University cooperates with Shaanxi, using heating crystallization method, prepares oversize monocrystalline perovskite CH for the first time3NH3PBI3, but its monocrystalline
Tank solution is needed to grow repeatedly, the growth large single crystal time is longer, and quality can be declined slightly.
Summary of the invention
In view of the drawbacks of the prior art, the purpose of the present invention is to provide a kind of preparation methods of perovskite monocrystalline, it is intended to
Solve nucleus quantity in existing perovskite method for preparing single crystal it is more lead to prepare perovskite monocrystalline time-consuming, quality is low and
The low technical problem of solution utilization rate.
A kind of preparation method of perovskite monocrystalline provided by the present invention, the molecular formula of perovskite are ABX3, including it is as follows
Step:
(1) it takes the first halide and the second halide to mix, and uses polar solvent stirring and dissolving, obtained perovskite solution,
The mass ratio of first halide, the second halide and polar solvent requires to make perovskite solution concentration close to saturation;
(2) perovskite solution is filtered processing;
(3) the perovskite solution for being filtered processing is placed in hydrophobic container, perovskite monocrystalline is precipitated in heating, dredges
Nucleus quantity reduces on water capacity wall, so that the unit growth rate of perovskite monocrystalline improves;
The molecular formula of first halide is AX, and the second halide molecule formula is BX2;A is methyl amine
(CH3NH3), caesium (Cs), carbonamidine (NH2CH=NH2) in a kind of or any two kinds of mixture or three kinds of mixture;B is lead
(Pb), tin (Sn);X can be iodine (I), bromine (Br), a kind of or any two kinds of mixture or three kinds of mixture in chlorine (Cl), the
The ratio between molal quantity and the molal quantity of X of one mixture are 1:1, and the ratio between molal quantity and the molal quantity of X of the second mixture are 1:2,
First mixture refers to by methyl amine, caesium, any two or three of carbonamidine of the mixture constituted, the second mixture refer to by
The mixture for the composition that any two or three of iodine, bromine, chlorine.
When solution reaches supersaturation, impurity, bubble and the chamber wall that nucleus mainly relies in perovskite solution are generated, when
Using hydrophobic container, due to the hydrophobicity of hydrophobic chamber wall, the nucleus number generated on hydrophobic chamber wall is sharply reduced, the list grown
Brilliant quantity is opposite to be reduced, and the crystal grown in the unit time is bigger, and broken grain quantity is reduced, and solution utilization rate gets a promotion, crystal
Quality significantly improves.
Further, further include cleaning hydrophobic container before step (3), remove the impurity in hydrophobic container, crystalline substance can be reduced
Karyogenesis quantity.
Further, step (3) successively cleans hydrophobic container with deionized water, acetone, isopropanol and deionized water, then uses
Nitrogen gun drying.
Further, perovskite solution is filtered using high speed centrifugation in step (2), greatly reduces experimental period, reaches
Tiny nucleus in solution is reduced, the utilization rate of perovskite solution is promoted.
Further, heating temperature is 60 DEG C~110 DEG C in step (3).
Further, hydrophobic container local environment relative humidity is less than 50%.
Further, hydrophobic container is polytetrafluoroethylene (PTFE) (PTFE), has stability good, at low cost, reusable.
Contemplated above technical scheme through the invention, compared with prior art, can obtain it is following the utility model has the advantages that
1, it proposes that hydrophobic container is used to replace conventional glass container as perovskite crystal growth container in the present invention, so that
Nucleus is reduced perovskite monocrystalline during the growth process, and the volume that monocrystalline is grown in the unit time is bigger, and quality is higher, perovskite
Solution utilization rate promoted.
2, using high speed centrifugation to the perovskite solution filtering of preparation and before perovskite solution is added to hydrophobic container
To hydrophobic cleaning container, impurity in perovskite solution can be removed, and tiny nucleus in solution can be reduced, enable solution
It is enough that more bulky perovskite monocrystalline are sucked out, improve the utilization rate of perovskite solution.
Detailed description of the invention
Fig. 1 is the flow chart of the preparation method of perovskite monocrystalline provided by the invention;
Fig. 2 is the comparison using the perovskite monocrystalline and the perovskite monocrystalline using glass container preparation of the preparation of PTFE container
Figure;
Fig. 3 is the MAPbI prepared using PTFE container3Monocrystalline core uses the MAPbI of glass container preparation3The fluorescence of monocrystalline
Analyze result;
Fig. 4 is the MAPbBr prepared using PTFE container3Monocrystalline core uses the MA PbBr of glass container preparation3Monocrystalline it is glimmering
Light analyzes result.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
The first embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic iodide amine (CH of 1.59g is weighed3NH3I, MAI) and 3.688g lead iodide (PbI2), it is dissolved in
The gamma-butyrolacton (GBL) of 10mL is stirred dissolution 12-24h at 60 DEG C, obtains perovskite solution;
(2) perovskite solution is filtered with 0.45 μm of filter;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be carefully placed in PTFE container, is placed on 100 DEG C of warm tables and adds
Heat makes solvent slow evaporation, and perovskite solution reaches supersaturation, and crystal precipitation is grown up, and 1cm or so size can be obtained after 3-5h
MAPbI3Monocrystalline.
When solution reaches supersaturation, generate on impurity, bubble and the chamber wall that nucleus mainly relies in perovskite solution,
When using hydrophobic container, due to the hydrophobicity of hydrophobic chamber wall, the nucleus number generated on hydrophobic chamber wall is sharply reduced, while right
Perovskite solution is filtered and cleans before perovskite solution is added to PTFE container to PTFE container, can reduce
The impurity of perovskite solution reduces nucleus generation quantity, reduces so that the monocrystalline quantity grown is opposite, grows in the unit time
Crystal is bigger, and broken grain quantity is reduced, and solution utilization rate gets a promotion, and crystal quality significantly improves.
The second embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic Diethylaminoethyl amine (CH of 1.12g is weighed3NH3Br, MABr) and 2.936g lead bromide (PbBr2),
It is dissolved in the n,N-Dimethylformamide (DMF) of 10mL, dissolution 12-24h is stirred at 60 DEG C, obtains perovskite solution;
(2) perovskite solution is filtered with 0.45 μm of filter;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be placed in PTFE container, is placed on 60 DEG C of warm tables and heats, make solvent
Slow evaporation, perovskite solution reach supersaturation, and crystal precipitation is grown up, and the MAPbBr of 1cm or so size can be obtained after 3-5h3
Monocrystalline.
The 3rd embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic Diethylaminoethyl amine (CH of 1.59g is weighed3NH3I) with 2.936g lead bromide (PbBr2), it is dissolved in
The n,N-Dimethylformamide (DMF) of 10mL is stirred dissolution 12-24h at 60 DEG C, obtains perovskite solution;
(2) perovskite solution is filtered with 0.45 μm of filter;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be placed in PTFE container, is placed on 60 DEG C of warm tables and heats, make solvent
Slow evaporation, perovskite solution reach supersaturation, and crystal precipitation is grown up, and 0.6cm or so size can be obtained after 3-5h
MAPbIBr2Monocrystalline.
The fourth embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic Diethylaminoethyl amine (CH of 1.12g is weighed3NH3Br) with 3.688g lead bromide (PbI2), it is dissolved in
The n,N-Dimethylformamide (DMF) of 10mL and the mixed solution of gamma-butyrolacton (GBL), n,N-Dimethylformamide and γ-fourth
The volume ratio of lactone is 2:8, and dissolution 12-14h is stirred at 60 DEG C, obtains perovskite solution;
(2) perovskite solution is obtained by filtration with 0.45 μm of filter;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be placed in PTFE container, is placed on 60 DEG C of warm tables and heats, make solvent
Slow evaporation, perovskite solution reach supersaturation, and crystal precipitation is grown up, and 0.6cm or so size can be obtained after 3-5h
MAPbI2Br monocrystalline.
5th embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic iodate carbonamidine (NH of 1.72g is weighed2CH=NH2I) with 3.688g lead iodide (PbI2), it is dissolved in
10mLGBL is stirred dissolution 12-24h at 60 DEG C, obtains perovskite solution;
(2) perovskite solution is filtered using high speed centrifugation;It can be improved the preparation of perovskite monocrystalline using high speed centrifugation
Rate, and the impurity in perovskite solution can be effectively reduced, reduce nucleus generation quantity;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be placed in PTFE container, is placed on 120 DEG C of warm tables and heats, make molten
Agent slow evaporation, perovskite solution reach supersaturation, and crystal precipitation is grown up, and 0.5cm or so size can be obtained after 3-5h
NH2CH=NH2PbI3Monocrystalline.
The sixth embodiment of the preparation method of perovskite monocrystalline provided by the invention, specific preparation process is as follows:
(1) the synthetic iodide amine (CH of 1.272g is weighed3NH3I), 0.344g iodate carbonamidine (NH2CH=NH2I)
With 3.688g lead bromide (PbBr2), it is dissolved in 10mLGBL, dissolution 12-24h is stirred at 60 DEG C, obtains perovskite solution.
(2) perovskite solution is filtered using high speed centrifugation;
(3) PTFE container 10min is cleaned with deionized water, cleans PTFE container 10min with acetone, is cleaned with isopropanol
PTFE container 10min cleans PTFE container 10min with deionized water, then is dried up with nitrogen gun;
(4) it takes the filtered perovskite solution of 10mL to be placed in PTFE container, is placed on 110 DEG C of warm tables and heats, make molten
Agent slow evaporation, perovskite solution reach supersaturation, and crystal precipitation is grown up, and 0.5cm or so size can be obtained after 3-5h
(CH3NH3)0.8(NH2CH=NH2I)0.2PbBr3Monocrystalline.
Perovskite monocrystalline 1 is to be made using preparation method provided by the invention in Fig. 2, is preparing perovskite solution,
It is placed in PTFE container, the perovskite monocrystalline 1 that heating is precipitated after two hours.Perovskite monocrystalline 2 to perovskite monocrystalline 4 is in Fig. 2
It is made using glass container, after preparing perovskite solution, is placed in glass container, the perovskite that heating is precipitated after two hours
Monocrystalline 2, the side length of perovskite monocrystalline 1 are about 0.8cm, and the side length of perovskite monocrystalline 2 is about 0.3cm, interior at the same time, are adopted
The volume of perovskite monocrystalline 1 made from PTFE container is far longer than using perovskite monocrystalline 2 made from glass container.It is placed in glass
Perovskite solution in glass container perovskite monocrystalline 3 obtained after 4 h of heating, volume is placed in again smaller than perovskite monocrystalline 1
Perovskite solution in glass container 4 volume of perovskite monocrystalline obtained after heating 6h is not grown up.It can be seen that using hydrophobic
Container prepares perovskite monocrystalline, reduces the quantity of nucleus, so that the volume for growing monocrystalline in the unit time is bigger, reduces broken
The utilization rate of crystalline substance, perovskite solution also improves.
Fig. 3 is that luminoscope prepares MAPbI to PTFE container3Monocrystalline and the MAPbI prepared with glass container3Monocrystalline quality
It detects, can see in figure, when wavelength is between 770nm~780nm, using the MAPbI of PTFE container preparation3It monocrystalline and adopts
The MAPbI prepared with glass container3The fluorescence intensity of monocrystalline reaches maximum, and using the MAPbI of PTFE container preparation3Monocrystalline
Fluorescence intensity be the MAPbI prepared using glass container33 times of the fluorescence intensity of monocrystalline.It can be seen that using PTFE container
Prepare MAPbI3Monocrystalline can significantly improve MAPbI3Monocrystalline quality.
Fig. 4 is that luminoscope prepares MAPbBr to PTFE container3Monocrystalline and the MAPbBr prepared with glass container3Monocrystalline
Amount detects, and can see in figure, when wavelength is between 535nm~545nm, using the MAPbI of PTFE container preparation3Monocrystalline
Fluorescence intensity is the MAPbI prepared using glass container35 times of the fluorescence intensity of monocrystalline.It can be seen that using PTFE container system
Standby MAPbBr3Monocrystalline can significantly improve MAPbBr3Monocrystalline quality.
As it will be easily appreciated by one skilled in the art that the foregoing is merely illustrative of the preferred embodiments of the present invention, not to
The limitation present invention, any modifications, equivalent substitutions and improvements made within the spirit and principles of the present invention should all include
Within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of perovskite monocrystalline, the molecular formula of perovskite is ABX3, which comprises the steps of:
(1) the first halide and the second halide are mixed, and uses polar solvent stirring and dissolving, obtained perovskite solution is described
The mass ratio of first halide, second halide and the polar solvent requires to make perovskite solution concentration close to saturation;
(2) the perovskite solution is filtered processing;
(3) the perovskite solution for being filtered processing is placed in hydrophobic container, perovskite monocrystalline, hydrophobic appearance is precipitated in heating
The hydrophobicity of device reduces nucleus quantity on hydrophobic chamber wall, realizes that the unit growth rate of perovskite monocrystalline improves;
The molecular formula of first halide is AX, and the second halide molecule formula is BX2;A is methyl amine, one in caesium, carbonamidine
Kind or any two kinds of mixture or three kinds of mixture;B is lead, tin;X can for iodine, bromine, a kind of or any two kinds mixed in chlorine
Close object or three kinds of mixture.
2. preparation method according to claim 1, which is characterized in that further include cleaning hydrophobic container before the step (3).
3. preparation method according to claim 2, which is characterized in that use deionized water, acetone, isopropanol and deionized water
Hydrophobic container is successively cleaned, then is dried up with nitrogen gun.
4. preparation method according to claim 1-3, which is characterized in that in the step (2) using high speed from
The heart filters perovskite solution.
5. preparation method according to claim 1-3, which is characterized in that heating temperature is in the step (3)
60 DEG C~110 DEG C.
6. preparation method according to claim 1-3, which is characterized in that the hydrophobic container local environment is opposite
Humidity is less than 50%.
7. preparation method according to claim 1-3, which is characterized in that the material of the hydrophobic container is poly- four
Vinyl fluoride.
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CN108950689B (en) * | 2017-05-19 | 2020-12-04 | 卫子健 | Method for preparing perovskite crystal |
TWI630293B (en) | 2017-05-19 | 2018-07-21 | 國立清華大學 | Method for preparing perovskite crystal |
CN107325004A (en) * | 2017-08-01 | 2017-11-07 | 苏州协鑫纳米科技有限公司 | Perovskite crystal and preparation method thereof |
CN107829139B (en) * | 2017-11-07 | 2020-09-22 | 西北工业大学 | Inverse temperature solution growth method of all-inorganic perovskite single crystal |
CN108559503B (en) * | 2018-03-30 | 2020-07-07 | 华中科技大学 | Cs (volatile organic Compounds)2AgBiBr6Double perovskite and preparation method thereof |
CN109920939B (en) * | 2019-02-01 | 2022-03-29 | 西交利物浦大学 | Solvent, method and application for preparing high-performance metal halide perovskite film |
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CN110294455A (en) * | 2019-06-26 | 2019-10-01 | 上海大学 | Functional material located growth method |
CN112746309B (en) * | 2020-12-25 | 2022-03-22 | 山东科技大学 | Preparation method and application of large-size perovskite single crystal with continuously adjustable cesium content |
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