CN105350078A - Method for rapid preparation of large-area perovskite crystals - Google Patents

Method for rapid preparation of large-area perovskite crystals Download PDF

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Publication number
CN105350078A
CN105350078A CN201510763073.0A CN201510763073A CN105350078A CN 105350078 A CN105350078 A CN 105350078A CN 201510763073 A CN201510763073 A CN 201510763073A CN 105350078 A CN105350078 A CN 105350078A
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perovskite crystal
solution
uhligite
big area
method preparing
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CN105350078B (en
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谢伟广
周洋洋
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Jinan University
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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
    • C30B29/16—Oxides
    • C30B29/22—Complex oxides
    • 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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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The invention belongs to the semiconductor optoelectronic material and device preparation technology field, and discloses a method for rapid preparation of large-area perovskite crystals. The method comprises the following steps: certain amounts of lead halide and methyl ammonium halide are weighed, mixing is carried out, then 1,4-butyrolactone, dissolving is carried out, and a perovskite solution is prepared; then the prepared perovskite solution is added to an organic solvent with a certain amount, and perovskite crystals are precipitated. Perovskite crystals are precipitated rapidly through a solution extraction mode, the method is simple and practical, the repeatability is high, external requirements are not high, different organic solvents can be selected for growth according to practical demands to obtain monocrystalline particles with different sizes, the maximum monocrystalline particle size can reach dozens of micron and thus the monocrystalline particles have great advantages at the aspect of manufacturing of photoelectric devices.

Description

A kind of quick method preparing big area perovskite crystal
Technical field
The invention belongs to Semiconductor Optoeletronic Materials and device preparing technical field, particularly a kind of quick method preparing big area perovskite crystal.
Background technology
Uhligite (CH 3nH 3pbI 3, CH 3nH 3pbCl 3, CH 3nH 3pbBr 3) material is due to its high uptake factor, bipolar transmission electron hole, cheapness and the advantage such as film deposition techniques and be widely used as solar cell active coating easily.Solar battery efficiency at present based on uhligite active coating reaches 20.1%.But, in uhligite active coating, the diffusion length of current carrier, life-span and mobility affect its key factor (SumTC as battery, MathewsN.Advancementsinperovskitesolarcells:photophysics behindthephotovoltaics [J] .Energy & EnvironmentalScience, 2014,7 (8): 2518-2534.), and these factors all with the crystallinity of active coating film and pattern closely related.Experiment shows that uhligite single grain size is larger, its carrier diffusion length is longer, less (the ShiD of defect state density, AdinolfiV, CominR, etal.Lowtrap-statedensityandlongcarrierdiffusioninorgano leadtrihalideperovskitesinglecrystals [J] .Science, 2015,347 (6221): 519-522.), these character make large size single crystal uhligite have larger advantage in making photoelectric device etc.
At present, perovskite crystal (CH is prepared 3nH 3pbI 3) mainly contain following several method: (1) is by controlling PbI 2crystal joins CH 3nH 3crystallization (YangS, ZhengYC, HouY, etal.FormationMechanismofFreestandingCH in I solution 3nH 3pbI 3functionalCrystals:InSituTransformationvsDissolution – Crystallization [J] .ChemistryofMaterials, 2014,26 (23): 6705-6710.); (2) by reverse solution vapor auxiliary law crystallization (ShiD, AdinolfiV, CominR, etal.Lowtrap-statedensityandlongcarrierdiffusioninorgano leadtrihalideperovskitesinglecrystals [J] .Science, 2015,347 (6221): 519-522.); (3) by the crystallization of reverse dissolution degree method (KadroJM, NonomuraK, GachetD, etal.FacileroutetofreestandingCH 3nH 3pbI 3crystalsusinginversesolubility [J] .ScientificReports, 2015,5.).Crystalline growth velocity prepared by these methods is comparatively slow, and productive rate is lower, is unfavorable for extensive preparation.In order to overcome the problems referred to above, need to find the method preparing big area perovskite crystal fast further.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art with not enough, the object of the present invention is to provide a kind of quick method preparing big area perovskite crystal.Perovskite crystal is separated out fast by the mode of solution extracting.
Object of the present invention is realized by following proposal:
The quick method preparing big area perovskite crystal, it comprises the following steps:
Take a certain amount of lead halide and methyl ammonium halide, mixing, adds GBL, dissolves, obtains uhligite solution; Then gained uhligite solution is added in a certain amount of organic solvent, separate out to obtain perovskite crystal.
Described lead halide can be lead chloride (PbCl 2), lead bromide (PbBr 2) and lead iodide (PbI 2) in any one;
Preferably, described lead halide is lead iodide (PbI 2);
Described methyl ammonium halide can be ammonio methacrylate (CH 3nH 3cl), methyl bromide ammonium (CH 3nH 3and methylpyridinium iodide ammonium (CH Br) 3nH 3i) any one in.
Preferably, described methyl ammonium halide is methylpyridinium iodide ammonium (CH 3nH 3i).
The mol ratio of lead halide used and methyl ammonium halide can be 1:1 ~ 3:1.
Preferably, the mol ratio of lead halide used and methyl ammonium halide is 1:1.
The concentration of described uhligite solution can be (0.5 ~ 1) mol/L.
Preferably, the concentration of described uhligite solution is 1mol/L.
Described dissolving can be heating for dissolving.
Preferably, described dissolving refers at 60 DEG C of heating for dissolving 1.5h.
Described organic solvent can be at least one in dimethyl silicone oil, dimethyl formamide, dimethyl sulfoxide (DMSO), ether and toluene.
Preferably, described organic solvent is at least one in dimethyl silicone oil, dimethyl formamide and ether.
The temperature of described organic solvent can be room temperature ~ 150 DEG C, because the abundant dissolution rate of different organic solvents and GBL is different, organic solvent can be made to mix rapidly with GBL by heating.
Uhligite solution used and the volume ratio of organic solvent are (5 ~ 15): (1000 ~ 2000).
Mechanism of the present invention is:
GBL dissolves the fine solvent of perovskite material, and be dissolved with in the GBL solution of uhligite and there is many uhligite colloids (size <100nm).If join in organic solvent by the GBL solution of solubilize calcium titanium ore, according to organic solvent similar dissolve mutually theory, GBL can extract by various organic solvent from uhligite solution, and remaining uhligite colloidal particle recrystallization is also grown up.After GBL is extracted completely, crystallographic dimension is just fixed up, and no longer continues recrystallization, because now do not had the solvent of solubilize calcium titanium ore colloidal particle.So the size of final crystallize out depends on that organic solvent extracts the speed of GBL, and the speed that different organic solvents extracts GBL is different, causes the size of growing crystal also different.
The present invention, relative to prior art, has following advantage and beneficial effect:
(1) method preparing perovskite crystal of the present invention's proposition is simple, reproducible, productive rate is high, and environment is as less demanding in humidity, temperature etc. to external world.
(2) by the quick growth uhligite single-crystal techniques that the present invention proposes, can obtain the single crystal particle of different size size, can select different organic solvent growths according to the actual requirements, this material is expected to obtain important application in fields such as photoelectric devices.
Accompanying drawing explanation
Fig. 1 is the X-ray diffractogram of the uhligite monocrystal material that uhligite solution grows respectively in dimethyl formamide, dimethyl silicone oil and ether.
Fig. 2 is scanning electron microscope (SEM) and the optics picture of the uhligite monocrystal material that uhligite solution grows respectively in dimethyl formamide, dimethyl silicone oil and ether.Wherein, the scanning electron microscope (SEM) of the uhligite monocrystal material that (a) (c) (e) in Fig. 2 grows in dimethyl silicone oil for uhligite solution and optics picture; Scanning electron microscope (SEM) photo of the uhligite monocrystal material that (b) in Fig. 2 grows in dimethyl formamide for uhligite solution; Scanning electron microscope (SEM) photo of the uhligite monocrystal material that (f) in Fig. 2 grows in diethyl ether solution for uhligite solution.
Embodiment
Below in conjunction with embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
In embodiment, agents useful for same all can be buied from market.
Embodiment 1
(1) by the PbI of 2.5mmol 2powder and 2.5mmolCH 3nH 3the vial of 5mL is put in the mixing of I powder, adds 2.5mL1,4-butyrolactone, to be placed in 60 DEG C of constant temperature ovens heated and stirred until powder dissolves completely after shaking up;
(2) get 1mL dimethyl silicone oil and be placed in 5mL beaker, the thermal station simultaneously beaker being placed on 150 DEG C heats;
(3) after in the first step vial, powder dissolves completely, get 10 μ L uhligite solution and join in dimethyl silicone oil, namely 30s forms the crystal of black at once.
The analyses of X-ray diffractogram spectrum analysis (as Fig. 1), SEM and optical photograph ((a), (c), (e) as in Fig. 2) are carried out to gained black crystals in embodiment 1, through confirming, the black crystals of growth is perovskite crystal material.
Embodiment 2
(1) by the PbI of 2.5mmol 2powder and 2.5mmolCH 3nH 3the glass cylinder bottle of 5mL is put in the mixing of I powder, adds 2.5mL1,4-butyrolactone, to be placed in 60 DEG C of constant temperature ovens heated and stirred until powder dissolves completely after shaking up;
(2) get in 2mL dimethyl formamide solution instillation 5mL beaker, the thermal station simultaneously beaker being placed on 70 DEG C heats;
(3) after in the first step glass cylinder, powder dissolves completely, get in the uhligite solution instillation dimethyl formamide solution of 5 μ L, namely 24s forms black crystals.
To gained black crystals in embodiment 2 carry out X-ray diffractogram spectrum analysis (as Fig. 1) and SEM take pictures ((b) as in Fig. 2) analyze, through confirming, the black crystals of growth is uhligite monocrystal material.
Embodiment 3
(1) by the PbI of 2.5mmol 2the CH of powder and 2.5mmol 3nH 3the glass cylinder bottle of 5mL is put in the mixing of I powder, adds 2.5mL1,4-butyrolactone, to be placed in 60 DEG C of constant temperature ovens heated and stirred until powder dissolves completely after shaking up;
(2) get in 1.5mL diethyl ether solution instillation 5mL beaker, beaker does not heat;
(3) after in the first step glass cylinder, powder dissolves completely, get in the uhligite solution instillation diethyl ether solution of 15 μ L, namely 26s forms black crystals.
To gained black crystals in embodiment 3 carry out X-ray diffractogram spectrum analysis (as Fig. 1) and SEM take pictures ((f) as in Fig. 2) analyze, through confirming, the black crystals of growth is uhligite monocrystal material.
From embodiment 1, can find out in embodiment 2 and embodiment 3, the preparation method of perovskite crystal provided by the invention, its crystal growth time is about 30s, substantially reduce crystal growth time, and wherein crystal grain sizes is maximum reaches tens micro-meter scales, make it in making photoelectric device etc., have larger advantage.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.

Claims (10)

1. prepare a method for big area perovskite crystal fast, it is characterized in that comprising the following steps: take a certain amount of lead halide and methyl ammonium halide, mixing, adds Isosorbide-5-Nitrae-Ding lactones, dissolves, obtains uhligite solution; Then gained uhligite solution is joined in a certain amount of organic solvent, separate out to obtain perovskite crystal.
2. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described lead halide is PbCl 2, PbBr 2and PbI 2in any one; Described methyl ammonium halide is CH 3nH 3cl, CH 3nH 3br and CH 3nH 3any one in I.
3. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described lead halide is PbI 2; Described methyl ammonium halide is CH 3nH 3i.
4. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described organic solvent is at least one in dimethyl silicone oil, dimethyl formamide, dimethyl sulfoxide (DMSO), ether and toluene.
5. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described organic solvent is at least one in dimethyl silicone oil, dimethyl formamide and ether.
6. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: the mol ratio of lead halide used and methyl ammonium halide is 1:1 ~ 3:1; The concentration of described uhligite solution is (0.5 ~ 1) mol/L.
7. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: the mol ratio of lead halide used and methyl ammonium halide is 1:1; The concentration of described uhligite solution is 1mol/L.
8. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: uhligite solution used and the volume ratio of organic solvent are (5 ~ 15): (1000 ~ 2000).
9. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described dissolving refers to heating for dissolving; The temperature of described organic solvent is normal temperature ~ 150 DEG C.
10. the quick method preparing big area perovskite crystal according to claim 1, is characterized in that: described dissolving refers at 60 DEG C of heating for dissolving 1.5h.
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CN106637403A (en) * 2016-11-28 2017-05-10 华中科技大学 Preparation method of perovskite single crystals
WO2018018481A1 (en) * 2016-07-28 2018-02-01 The University Of Hong Kong Fabrication of perovskite periodic arrays for optoelectronic applications
CN108560056A (en) * 2018-05-17 2018-09-21 武汉大学 A kind of two dimension perovskite monocrystal material and preparation method thereof
CN108987588A (en) * 2018-07-24 2018-12-11 南京信息工程大学 Multiple groups part perovskite absorbed layer precursor solution and preparation method thereof
CN110552061A (en) * 2019-09-16 2019-12-10 武汉大学 Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature
CN112981538A (en) * 2021-02-04 2021-06-18 广西大学 Method for growing large-size perovskite single crystal
US11186890B2 (en) 2016-08-24 2021-11-30 The University Of Hong Kong Two-phase steel and method for the fabrication of the same
CN113845428A (en) * 2021-09-10 2021-12-28 中国科学院上海光学精密机械研究所 Preparation method of perovskite material powder

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WO2018018481A1 (en) * 2016-07-28 2018-02-01 The University Of Hong Kong Fabrication of perovskite periodic arrays for optoelectronic applications
CN109906288A (en) * 2016-07-28 2019-06-18 香港大学 The preparation of perovskite cyclic array for photovoltaic applications
CN109906288B (en) * 2016-07-28 2021-03-09 香港大学 Preparation of periodic arrays of perovskites for photovoltaic applications
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US11186890B2 (en) 2016-08-24 2021-11-30 The University Of Hong Kong Two-phase steel and method for the fabrication of the same
CN106637403A (en) * 2016-11-28 2017-05-10 华中科技大学 Preparation method of perovskite single crystals
CN106637403B (en) * 2016-11-28 2019-04-12 华中科技大学 A kind of preparation method of perovskite monocrystalline
CN108560056A (en) * 2018-05-17 2018-09-21 武汉大学 A kind of two dimension perovskite monocrystal material and preparation method thereof
CN108987588A (en) * 2018-07-24 2018-12-11 南京信息工程大学 Multiple groups part perovskite absorbed layer precursor solution and preparation method thereof
CN110552061A (en) * 2019-09-16 2019-12-10 武汉大学 Preparation method for growing perovskite single crystal by liquid-phase diffusion separation crystallization at room temperature
CN112981538A (en) * 2021-02-04 2021-06-18 广西大学 Method for growing large-size perovskite single crystal
CN113845428A (en) * 2021-09-10 2021-12-28 中国科学院上海光学精密机械研究所 Preparation method of perovskite material powder

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