CN110318093A - A method of efficiently preparing hybrid inorganic-organic perovskite seed crystal - Google Patents
A method of efficiently preparing hybrid inorganic-organic perovskite seed crystal Download PDFInfo
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- CN110318093A CN110318093A CN201910361384.2A CN201910361384A CN110318093A CN 110318093 A CN110318093 A CN 110318093A CN 201910361384 A CN201910361384 A CN 201910361384A CN 110318093 A CN110318093 A CN 110318093A
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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
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Abstract
The present invention relates to crystallography fields, more particularly to a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal, the technical problem to be solved is that provide a kind of method for preparing hybrid inorganic-organic perovskite seed crystal using hydrogen ion induced growth, the seed crystal of high quality can efficiently be prepared by this method, easily controllable simultaneously, seed crystal obtained is convenient for storage；The technical solution of use are as follows: perovskite seed crystal is prepared using inversion crystallisation, adjust hydrogen ion concentration in perovskite crystal growth liquid, reduce pH value 0.5-4, to achieve the purpose that induce perovskite seed crystal fast-growth, acid is introduced into perovskite presoma growth-promoting media by the present invention, and the formation time and quantity of perovskite seed crystal are controlled by the range of adjusting pH, substantially reduce the time of seeded growth.
Description
Technical field
The present invention relates to crystallography fields, and in particular to a kind of side for efficiently preparing hybrid inorganic-organic perovskite seed crystal
Method.
Background technique
In recent years, since energy problem gets worse, there is an urgent need to look for the new energy or change current energy by people
Source structure.A kind of to be emerged silently based on the solar battery that perovskite is light-absorption layer, a few years, authentication efficiency is
Reach 22.7%.Currently, people are more to be concerned with how to improve the stability of its film, improve its photoelectric conversion efficiency
Deng, but its relevant mechanism study is but very lacked.Researcher should be more the basic nature for paying close attention to perovskite
Matter and principle, this is improved to the efficiency of perovskite battery and the discovery of new material has important meaning.And monocrystalline is due to it
The advantages that periodic regular arrangement, no crystal boundary is the first choice for carrying out mechanism study.And the seed crystal of high quality is to obtain research grade
The premise of large size single crystal.
Solwution method, which prepares perovskite monocrystalline common method, to be had: evaporative crystallization, decrease temperature crystalline, anti-solvent assisting crystallisation and inversion
It crystallizes (retrograde solubility crystallization), inversion crystallisation has the advantages such as growth cycle is short, and crystalline quality is good relative to other methods, more
Add and is suitble to growth monocrystalline.Existing patent CN106283195A describes inversion crystallisation and prepares hybrid inorganic-organic perovskite list
Crystalline substance, although the crystal growth period is short, there are its monocrystalline is of poor quality, it is harsh to equipment requirement the defects of；Patent
201810640065.0 disclose a kind of method that photoinduction prepares large-size high-quality hybrid inorganic-organic perovskite monocrystalline,
But it is more demanding to the control of light, in perovskite crystal growth liquid during seeded growth, absorption due to solution to light,
And the reason of variable density light intensity is constantly changing, therefore illumination is not easy to control, while monocrystalline obtained needs are protected from light guarantor
It deposits, preserving type is harsher.Therefore a kind of simple easily controllable and operation hybrid inorganic-organic perovskite list of induction is needed
The method of crystalline substance preparation.
Summary of the invention
The invention overcomes the deficiencies of the prior art, and provides it is a kind of using hydrogen ion induced growth prepare it is organic-
The seed crystal of high quality can efficiently be prepared by the method for inorganic hybridization perovskite seed crystal, this method, while easily controllable, be made
Seed crystal convenient for storage.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention are as follows: a kind of efficiently to prepare hybrid inorganic-organic
The method of perovskite seed crystal, the molecular formula of perovskite are ABX3, perovskite seed crystal is prepared using inversion crystallisation, adjusts perovskite
Hydrogen ion concentration in crystal growth liquid reduces pH value 0.5-4, to achieve the purpose that induce perovskite seed crystal fast-growth.
Specifically efficiently prepare hybrid inorganic-organic perovskite seed crystal method the following steps are included:
(1) two kinds of compounds of Y and Z are mixed according to a certain percentage, and is dissolved with solvent；
(2) above-mentioned configured perovskite crystal growth liquid is filtered processing；
(3) acid will be added in above-mentioned filtered solution, reduces pH value 0.5-4；It is then placed in container and seals, and heat
It is kept the temperature to certain temperature, perovskite monocrystalline ABX is precipitated3；
(4) it rinses, is dried up to get the perovskite seed crystal of high quality is arrived after taking out seed crystal.
The A is CH3NH3 +, NH=CHNH3 +, (CH3)4N+, C7H7 +, C3H11SN2+, C4H9NH3 2+, NH3C6H4CoCH3 2+Or
(NH2C3H2NSCH3)2+One of or it is a variety of, the B be Pb2+, Ge2+Or Sn2+One of or it is a variety of, the X be Br-, Cl-
Or I-One of or it is a variety of.
The Y is halides, specifically: chloromethane amine, bromine methylamine, iodine methylamine, chloromethane amidine, bromine carbonamidine, iodine carbonamidine, chlorination four
Methylamine, bromination tetramethylammonium, iodate tetramethylammonium, benzyl chloride, cylite, iodate benzyl, chloro 2- isothiourea, bromo 2- isothiourea, iodine
For one of 2- isothiourea or a variety of mixing.
The Z is halides, specifically: stannous chloride, tin tetrachloride, stannous bromide, stannous iodide, lead chloride, bromination
Lead, lead iodide, lead acetate, germanium chloride, one of bromination germanium or iodate germanium or a variety of mixing.
The Y and Z is mixed with the molar ratio of 1:1~5, and the solvent is n-methyl-2-pyrrolidone, N-N diformazan
Base formamide, 1,4-butyrolactone, dimethyl sulfoxide, chlorobenzene, acetonitrile, N-Methyl pyrrolidone, one of methylene chloride or more
The mixing of kind.
The temperature kept the temperature in the step (3) is 45-135 DEG C.
The acid being added in the step (3) is hydroiodic acid, hydrobromic acid, hydrochloric acid, acetic acid, phosphoric acid, oleic acid, oxalic acid, sulfurous acid,
Dilute sulfuric acid, metasilicic acid, hydrogen cyanide, carbonic acid, hydrosulphuric acid, hypochlorous one or more mixing.Due to hybrid inorganic-organic calcium
The content of colloid has substantial connection in the precipitation of titanium ore monocrystalline and solution, and the quick dissociation of colloid will lead to crystal and analyse faster
Out, and the presence of acid can accelerate the dissociation of colloid in solution, therefore the present invention using hydrogen ion as seeded growth induction because
Element.
The preferred acid is hydroiodic acid, hydrobromic acid, hydrochloric acid.The addition of these three acid not only introduces H ion, simultaneously
Corresponding halogen is introduced, the growth of monocrystalline is more conducive to.Meanwhile strong acid also has more more H ions.
The present invention has the advantages that compared with prior art.
1, acid is introduced into perovskite presoma growth-promoting media by first passage of the present invention, and is controlled by the range of adjusting pH
The formation time and quantity of perovskite seed crystal processed, substantially reduce the time of seeded growth.
2, the present invention in perovskite precursor solution by adding acid, so that perovskite seed crystal is precipitated, and obtain
The quality of perovskite seed crystal is substantially better than the seed crystal that conventional method obtains, and greatly improves the preparation yield of monocrystalline.
3, the present invention is used as inducer using acid, easily controllable during the preparation process, and convenient for operation, wants to Preparation equipment
It asks low, reduces production cost.
4, the quality of seed crystal produced by the present invention more preferably, with better light resistance, is stablized more preferably, is not required to be protected from light guarantor
It deposits, the cost of transport can be reduced.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, right below in conjunction with table and embodiment
The present invention is further elaborated.It should be appreciated that specific implementation example described herein is only used to explain the present invention,
It is not intended to limit the present invention.Embodiment institute is to analyze pure, iodide amine (CH using drug3NH3I) it is purchased from the big benefit of Australia
Sub- Dysol company；Acetic acid, hydroiodic acid and hydrochloric acid etc. are purchased from lark prestige Science and Technology Ltd.；Remaining drug is purchased from Chinese medicines group
Chemical reagent Co., Ltd.All material directly uses, without being further purified.
Case of comparative examples:
Accurately weigh 1.86g iodine methylamine (CH3NH3I) with 5.46g lead iodide (PbI2).By two kinds of raw material mixed dissolutions in
In the gamma-butyrolacton (GBL) of 9.6ml, stirring is sealed at 60 DEG C, it can ultrasound acceleration dissolution.After completely dissolution, aperture is used
0.45 μm of polytetrafluoroethylene filter filtering, is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set
It is 110 DEG C.Sealed glass jars equipped with precursor solution are placed in oil bath pan and are kept the temperature, after 180min, have a large amount of crystal to be precipitated.
Seed crystal is taken out drying to save.
Embodiment 1:
Accurately weigh 1.86g iodine methylamine (CH3NH3I) with 5.46g lead iodide (PbI2).By two kinds of raw material mixed dissolutions in
In the gamma-butyrolacton (GBL) of 9.6ml, stirring is sealed at 60 DEG C, it can ultrasound acceleration dissolution.After completely dissolution, to growth-promoting media
The acetic acid of the middle hydrochloric acid that 30 μ L are added dropwise and 20 μ L, stirs to clarify, and is filtered with 0.45 μm of the polytetrafluoroethylene filter in aperture,
It is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set as 110 DEG C.The sealing glass of precursor solution will be housed
Glass bottle, which is placed in oil bath pan, to be kept the temperature, and after 30min, has a large amount of crystal to be precipitated.Seed crystal is taken out drying to save.
Embodiment 2:
Accurately weigh 0.35g chloromethane amine (CH3NH3Cl) with 1.41g lead chloride (PbCl2).By two kinds of raw material mixed dissolutions in
In the dimethyl sulfoxide (DMSO) of 5ml and the chlorobenzene (CN) of 2ml, sealing stirring at normal temperature can ultrasound acceleration dissolution.It is sufficiently molten
The hydrochloric acid of 30 μ L and the acetic acid of 20 μ L are added dropwise into growth-promoting media, stirs to clarify by Xie Hou, with 0.45 μm of the polytetrafluoroethylene (PTFE) in aperture
Filter filtering, is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set as 60 DEG C.It will be molten equipped with forerunner
The sealed glass jars of liquid, which are placed in oil bath pan, to be kept the temperature, and after 60min, has a large amount of crystal to be precipitated.Seed crystal is taken out drying and saved and is
It can.
Embodiment 3:
Accurately weigh 0.75g bromine methylamine (CH3NH3Br) with 2.22g lead bromide (PbBr2).By two kinds of raw material mixed dissolutions in
In the n,N-Dimethylformamide (DMF) of 6ml, sealing stirring at normal temperature can ultrasound acceleration dissolution.After completely dissolution, Xiang Sheng
The oleic acid of 30 μ L is added dropwise in long liquid, stirs to clarify, is filtered with 0.45 μm of the polytetrafluoroethylene filter in aperture, is placed in sealing
In vial.Oil bath equipment is got out, oil bath temperature is set as 70 DEG C.Sealed glass jars equipped with precursor solution are placed in oil bath
It is kept the temperature in pot, after 50min, there is a large amount of crystal to be precipitated.Seed crystal is taken out drying to save.
Embodiment 4:
Accurately weigh 0.28g bromine methylamine (CH3NH3), Br 0.17g methylamine hydrochloride (CH3NH3) and 1.83g lead bromide Cl
(PbBr2).By three kinds of raw material mixed dissolutions in the n,N-Dimethylformamide (DMF) of 5ml, sealing stirring at normal temperature can
Ultrasound accelerates dissolution.After completely dissolution, the hydroiodic acid of 20 μ L is added into growth-promoting media, stirs to clarify, with 0.45 μm of aperture
Polytetrafluoroethylene filter filtering, is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set as 50 DEG C.It will
Sealed glass jars equipped with precursor solution, which are placed in oil bath pan, to be kept the temperature, and after 60min, has a large amount of crystal to be precipitated.Seed crystal is taken out
Drying saves.
Embodiment 5:
Accurately weigh 0.14g bromine methylamine (CH3NH3) and 0.36g lead chloride (PbCl Br2).By two kinds of raw material mixed dissolutions in
The N-Methyl pyrrolidone (NMP) of 4ml, in the dimethyl sulfoxide (DMSO) of 1.5ml and the chlorobenzene (CN) of 0.8ml, at normal temperature
Sealing stirring, can ultrasound acceleration dissolution.After completely dissolution, the phosphoric acid of 40 μ L is added dropwise into growth-promoting media, stirs to clarify, uses aperture
0.45 μm of polytetrafluoroethylene filter filtering, is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set as
45℃.Sealed glass jars equipped with precursor solution are placed in oil bath pan and are kept the temperature, after 70min, have a large amount of crystal to be precipitated.By seed
Crystalline substance takes out drying and saves.
Embodiment 6:
Accurately weigh 1.72g iodine carbonamidine (NH=CHNH3) and 4.61g lead iodide (PbI I2).By two kinds of raw material mixed dissolutions
In the gamma-butyrolacton (GBL) of 10ml, stirring is sealed at 50 DEG C, it can ultrasound acceleration dissolution.After completely dissolution, to growth-promoting media
The hydrochloric acid of the middle hydroiodic acid that 80 μ L are added dropwise and 20 μ L, stirs to clarify, and is filtered with 0.45 μm of the polytetrafluoroethylene filter in aperture,
It is placed in the vial of sealing.Oil bath equipment is got out, oil bath temperature is set as 110 DEG C.The sealing glass of precursor solution will be housed
Glass bottle, which is placed in oil bath pan, to be kept the temperature, and after 45min, has a large amount of crystal to be precipitated.Seed crystal is taken out drying to save.
Embodiment 7:
Accurately weigh 1.59g bromine methylamine (CH3NH3) and 2.936g lead iodide (PbI Br2).By two kinds of raw material mixed dissolutions in
In the N-N dimethylformamide (DMF) of 10ml, stirring is sealed at 60 DEG C, it can ultrasound acceleration dissolution.After completely dissolution, Xiang Sheng
The hydrosulphuric acid of 150 μ L is added in long liquid, stirs to clarify, is filtered, is placed in close with 0.45 μm of the polytetrafluoroethylene filter in aperture
In the vial of envelope.Oil bath equipment is got out, oil bath temperature is set as 60 DEG C.Sealed glass jars equipped with precursor solution are placed in
It is kept the temperature in oil bath pan, after 60min, there is a large amount of crystal to be precipitated.Seed crystal is taken out drying to save.
According to case of comparative examples and embodiment 1-7, the table that following crystal is precipitated pH variation with the time is precipitated is obtained.
| Embodiment | Control | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| PH variation | 0 | -1.5 | -2 | -0.8 | -1 | -2 | -1.8 | -3.2 |
| It is precipitated time (min) | 180 | 30 | 60 | 50 | 60 | 70 | 45 | 60 |
Wherein in pH variation, "-" refer to the solution in embodiment when not acid adding compared with the pH value of solution, the value of reduction.
Seed crystal obtained in above-mentioned case of comparative examples and embodiment 1, fluorescence spectra can be seen that use by above table
Its spectrogram of seed crystal made from adjusting pH value is more stable, and the fluorescence intensity of 1 seed crystal of embodiment is twice of case of comparative examples, hence it is evident that
Using the negligible amounts of seed crystal non-composite defect made from the method for adjusting forerunner's growth-promoting media pH value, the quality of monocrystalline is higher.
Above embodiment is merely exemplary to illustrate the principle of the present invention and its effect, and is not intended to limit the present invention.For
Person skilled in the art all without departing from the spirit and scope of the present invention, modifies above-described embodiment or is improved.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by tool usually intellectual in all act technical fields
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (9)
1. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal, the molecular formula of perovskite is ABX3, using inversion
Crystallisation prepares perovskite seed crystal, it is characterised in that: adjusts hydrogen ion concentration in perovskite crystal growth liquid, reduces pH value 0.5-
4, to achieve the purpose that induce perovskite seed crystal fast-growth.
2. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 1, feature exist
In, comprising the following steps:
(1) two kinds of compounds of Y and Z are mixed according to a certain percentage, and is dissolved with solvent；
(2) above-mentioned configured perovskite crystal growth liquid is filtered processing；
(3) acid will be added in above-mentioned filtered solution, reduces pH value 0.5-4；It is then placed in container and seals, and be heated to one
Determine temperature to be kept the temperature, perovskite monocrystalline ABX is precipitated3；
(4) it rinses, is dried up to get the perovskite seed crystal of high quality is arrived after taking out seed crystal.
3. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 1, feature exist
In the A is CH3NH3 +, NH=CHNH3 +, (CH3)4N+, C7H7 +, C3H11SN2+, C4H9NH3 2+, NH3C6H4CoCH3 2+Or
(NH2C3H2NSCH3)2+One of or it is a variety of, the B be Pb2+, Ge2+Or Sn2+One of or it is a variety of, the X be Br-, Cl-
Or I-One of or it is a variety of.
4. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 2, feature exist
In, the Y is halides, specifically: chloromethane amine, bromine methylamine, iodine methylamine, chloromethane amidine, bromine carbonamidine, iodine carbonamidine, tetramethylamine chloride,
Bromination tetramethylammonium, iodate tetramethylammonium, benzyl chloride, cylite, iodate benzyl, chloro 2- isothiourea, bromo 2- isothiourea, iodo 2- are different
One of thiocarbamide or a variety of mixing.
5. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 2, feature exist
In, the Z is halides, specifically: stannous chloride, tin tetrachloride, stannous bromide, stannous iodide, lead chloride, lead bromide, iodine
Change lead, lead acetate, germanium chloride, one of bromination germanium or iodate germanium or a variety of mixing.
6. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 2, feature exist
In the Y and Z are mixed with the molar ratio of 1:1~5, and the solvent is n-methyl-2-pyrrolidone, N-N dimethyl formyl
Amine, 1,4-butyrolactone, dimethyl sulfoxide, chlorobenzene, acetonitrile, N-Methyl pyrrolidone, one of methylene chloride or a variety of mixed
It closes.
7. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 2, feature exist
In the temperature kept the temperature in the step (3) is 45-135 DEG C.
8. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 2, feature exist
In the acid being added in the step (3) is hydroiodic acid, hydrobromic acid, hydrochloric acid, acetic acid, phosphoric acid, oleic acid, oxalic acid, sulfurous acid, dilute sulphur
Acid, metasilicic acid, hydrogen cyanide, carbonic acid, hydrosulphuric acid, hypochlorous one or more mixing.
9. a kind of method for efficiently preparing hybrid inorganic-organic perovskite seed crystal according to claim 8, feature exist
In the acid is hydroiodic acid, hydrobromic acid, one of hydrochloric acid or a variety of mixing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111341914A (en) * | 2020-03-23 | 2020-06-26 | 成都新柯力化工科技有限公司 | Adhesive flexible perovskite photovoltaic cell film and preparation method thereof |
| CN112251815A (en) * | 2020-09-11 | 2021-01-22 | 扬州大学 | One-dimensional DMAPbI3Method for growing large single crystal |
| CN114150363A (en) * | 2021-12-13 | 2022-03-08 | 吉林大学 | Growth method of tin-based perovskite single crystal |
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2019
- 2019-04-30 CN CN201910361384.2A patent/CN110318093A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111341914A (en) * | 2020-03-23 | 2020-06-26 | 成都新柯力化工科技有限公司 | Adhesive flexible perovskite photovoltaic cell film and preparation method thereof |
| CN112251815A (en) * | 2020-09-11 | 2021-01-22 | 扬州大学 | One-dimensional DMAPbI3Method for growing large single crystal |
| CN112251815B (en) * | 2020-09-11 | 2022-07-05 | 扬州大学 | One-dimensional DMAPbI3Method for growing large single crystal |
| CN114150363A (en) * | 2021-12-13 | 2022-03-08 | 吉林大学 | Growth method of tin-based perovskite single crystal |
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