CN106631816A - Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping - Google Patents

Preparation method of atomic-scale thickness two-dimensional perovskite nanosheet by liquid phase stripping Download PDF

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CN106631816A
CN106631816A CN201611206573.5A CN201611206573A CN106631816A CN 106631816 A CN106631816 A CN 106631816A CN 201611206573 A CN201611206573 A CN 201611206573A CN 106631816 A CN106631816 A CN 106631816A
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CN106631816B (en
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何海平
甘露
苏斌斌
叶志镇
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Zhejiang University ZJU
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Abstract

The invention discloses a preparation method of atomic-scale thickness two-dimensional perovskite nanosheet. A liquid phase stripping method is utilized; particularly, a two-dimensional perovskite block material is prepared by an intrastratal solution method; then an ultrasound assistant stripping method is used; the two-dimensional perovskite block liquid phase is stripped to be the atomic-scale thickness nanosheets by using the stripping liquid with relatively low polarity under the gentle stripping condition. The preparation method is convenient and easy to practice; the thickness of the acquired two-dimensional perovskite nanosheet can be maintained among at least several atomic layers of a single layer.

Description

A kind of liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet
Technical field
The present invention relates to a kind of liquid phase strip preparation method of two-dimentional perovskite nanometer sheet, obtained nanometer sheet has individual layer To the ultrathin of a few atomic layer.
Background technology
Two-dimensional material refer to electronics only can on the non-nanosize of two dimensions free movement (plane motion) material, Typical two-dimensional structure has nanometer sheet, superlattices, SQW etc..It is numerous solely that the quantum confinement characteristic of two-dimensional material imparts it Special physicochemical properties, such as plane conductivity, magnetic anisotropy, regulatable band structure and chemical mobility of the surface etc., It is set to possess huge application potential in numerous areas such as catalysis, energy storage, biology, photoelectricity.When two-dimentional block materials are by certain When method peels off into the ultra-thin materials of individual layer or several atomic layer level thickness, the specific surface area of jumbo increase not only increases material The physics and chemism on material surface, also affects the two-dimentional wave function caused because of quantum confined effect.Therefore, it is possible to pass through electricity Energy subband regulates and controls to modify the physical property of two-dimensional ultrathin material.With the day by day maturation of lift-off technology, various two are had at present Dimension material is successfully able to be separated into independent nano flake, such as Graphene (Graphene), transient metal sulfide (TMDs), Metal-organic framework material (MOFs) etc., they show excellent physicochemical characteristics.
Researcher has carried out various methods and has attempted that two-dimentional block materials are peeled off into the nano flake of atomic-level thickness, liquid phase Stripping is one of main method.Liquid phase peel off be in certain medium by ultrasonic means by two-dimensional ultrathin nanometer sheet from It is stripped out in respective masses material, the method so as to obtain the colloidal solution of two-dimensional ultrathin nanometer sheet.It is (molten by stripping media Agent and auxiliary reagent) screening can effectively improve the charge stripping efficiency of nanometer sheet.Liquid phase is peeled off and can in a large number, uniformly obtained because of it Obtain two-dimensional ultrathin nanometer sheet and be widely studied, a kind of more ripe stripping means has nowadays been become.At present, main liquid Phase stripping method has：Ion insertion, ion-exchange and ultrasonic wave added stripping method.
In recent years, a kind of organic and inorganic lead halide perovskite-like material because its low-defect-density, high carrier mobility, Luminous efficiency and strong light absorption ability and possess excellent photoelectric properties, and become nowadays burning hot photovoltaic material.It is short 5th, between 6 years, lifted to 22.1% from 3.8% based on the photoelectric transformation efficiency of the solar cell of this perovskite-like.
Preferably perovskite structure is cubic crystal structure, by common summit MX6Octahedron is constituted, and it is in three-dimensional unlimited extension Network structure is formed, the less atom of radius or molecule A are located in octahedral interstice.For three-dimensional organic and inorganic perovskite material Material, M is typically a kind of divalent metal atom, and X represents halogen atom, and wherein metal cation M is located at octahedra center, and less Organic molecule A (usually methylamine) be filled in the dodecahedron gap that six adjacent octahedrons are surrounded, general structure is AMX3.And when organic cation molecular chain length is larger, so that it may A is formed respectively according to organic cation valence state2MX4(A is+1 Valency) or AMX4The two-dimensional layer perovskite-like structure of (A is+divalent) two kinds of forms, wherein A positions cation is generally RNH3 +Or NH3RNH3 2+(R is alkyl or aryl radical).Research shows, when for R being alkyl, organic moiety C atom number Structure Transformation of the perovskite from three-dimensional to two dimension occurs when more than 3, and when R is aryl radical, organic moiety master Chain C atoms number can also form two-dimensional layered structure when being less than 3, such as (C6H5C2H4)2PbX4。
For two-dimentional AMX4Type perovskite, with hydrogen bond N-H's ... X between its organic cation and inorganic halides anion Mode is combined, and is combined by Van der Waals force between adjacent organic molecule chain, i.e., each atomic binding forces is more than layer in calcium titanium ore bed Between adhesion, but at present, there is no liquid phase stripping method to prepare the report of the two-dimentional perovskite ultrathin nanometer piece of atomic-level thickness.
The content of the invention
It is an object of the invention to provide a kind of side that atomic-level thickness two dimension perovskite nanometer sheet is prepared based on liquid phase stripping Method, the method is the profit by the architectural characteristic of atomic-level thickness two-dimensional material in combination with the excellent photoelectric properties of perovskite material Liquid phase lift-off technology is used, the ultra-thin preparation of two-dimentional perovskite is realized, the two-dimentional perovskite nanometer sheet of atomic-level thickness is obtained.
The preparation method of the atomic-level thickness two dimension perovskite nanometer sheet of the present invention, uses ultrasonic wave added stripping method, Specifically include following steps：
1) in an inert atmosphere, metal halide powder is added in test tube, ferrule will be tried, by syringe into test tube Add halogen acids to dissolve above-mentioned powder, then absolute methanol solution is injected as cushion on the upper strata of solution, finally by injection Liquid organic amine needed for device injection reaction, described organic amine and the mol ratio of metal halide is 2:1；Halogen acids and methyl alcohol It is excessive；
2) by Jing steps 1) process reactant liquor stand at least 2 week, cushion separate out flat crystal, will separate out sheet Crystal takes out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) flat crystal that vacuum drying is obtained is dispersed in low polarity stripper in the ratio of 1mg/ml, in gentle condition Under it is ultrasonically treated, you can obtain the two-dimentional perovskite nanometer sheet suspension of atomic-level thickness.
Above-mentioned inert atmosphere is reached by glove box, and oxygen content, water content are respectively less than 0.5ppm in glove box.
Above-mentioned metal halide is lead halide PbX2, halogen acids is HX, and wherein X is Br or I.
Above-mentioned liquid organic amine is phenyl ethylamine, and molecular formula is C6H5C2H4NH3。
The big flat crystal of above-mentioned precipitation is two-dimentional perovskite block stratified material, and molecular formula is (C6H5C2H4)2PbX4, its Middle X is Br or I.Have document to show, (C6H5C2H4NH3)2PbX4Individual layer atomic thickness is in 1.75nm or so.
Method used by the inventive method mainly contains two steps.The first step is that layer solwution method prepares two-dimentional perovskite block Body material.Second step for block materials liquid phase stripping process, be the main body step of this method, the pattern of the nanometer sheet of formation, Thickness is controlled by the reaction.Two-dimentional its thickness of perovskite nanometer sheet that the present invention is obtained can maintain individual layer to several Between individual atomic layer.
In course of reaction of the present invention, stripper adopts toluene solution, is the strong ion characteristic due to perovskite material, peels off The polarity of liquid is no more than ether.
In course of reaction of the present invention, using gentle ultrasound condition be due to the mechanical fragility of two-dimentional perovskite material, Violent ultrasound condition easily causes the organic fraction of two-dimentional perovskite to rupture.Described temperate condition typically refer to power 60～ 240W, ultrasonic 5～30min of duration.
Ultrasonic wave added peels off the method for preparing two-dimentional perovskite nanometer sheet, and to external world environment, equipment etc. require low, preparation ten Divide simplicity.
Description of the drawings
Fig. 1 is atomic force microscopy Electronic Speculum (AFM) photo of atomic-level thickness two dimension perovskite nanometer sheet.
Specific embodiment
Embodiment 1
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.367g PbBr2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HBr solution to dissolve PbBr by syringe2Powder, then pass through syringe on the upper strata of solution Add 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) process reactant liquor stand 2 week, a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbBr4Flat crystal is dispersed in toluene in the ratio of 1mg/ml In, the ultrasound 5min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbBr4Nanometer sheet suspends Liquid.
By (the C for preparing6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) is characterized, and nanometer sheet pattern keeps complete quadrangle, nanometer sheet thickness to be about 4.5nm.
Embodiment 2
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.367g PbBr2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HBr solution to dissolve PbBr by syringe2Powder, then pass through syringe on the upper strata of solution Add 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) process reactant liquor stand 2 week, a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbBr4Flat crystal is dispersed in toluene in the ratio of 1mg/ml In, the ultrasound 30min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbBr4Nanometer sheet suspends Liquid.
By (the C for preparing6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) is characterized, and nanometer sheet pattern is different, and complete quadrangle, nanometer sheet thickness can not have been kept to be about 3.7nm。
Embodiment 3
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.367g PbBr2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HBr solution to dissolve PbBr by syringe2Powder, then pass through syringe on the upper strata of solution Add 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) process reactant liquor stand 2 week, a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbBr4Flat crystal is dispersed in toluene in the ratio of 1mg/ml In, the ultrasound 30min under the ultrasonic power of 240W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbBr4Nanometer sheet is hanged Supernatant liquid.
By (the C for preparing6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) is characterized, and nanometer sheet pattern is different, and complete quadrangle, nanometer sheet thickness can not have been kept to be about 1.9nm。
Embodiment 4
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.461g PbI2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HI solution to dissolve PbI by syringe2Powder, then added by syringe on the upper strata of solution Enter 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) reactant liquor that processes stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in toluene in the ratio of 1mg/ml, The ultrasound 5min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
By (the C for preparing6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The micro- Electronic Speculum (AFM) of sub- power characterizes, and nanometer sheet pattern keeps complete quadrangle, nanometer sheet thickness to be about 5.1nm.
Embodiment 5
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.461g PbI2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HI solution to dissolve PbI by syringe2Powder, then added by syringe on the upper strata of solution Enter 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) reactant liquor that processes stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in toluene in the ratio of 1mg/ml, The ultrasound 30min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
By (the C for preparing6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The micro- Electronic Speculum (AFM) of sub- power characterizes, and nanometer sheet pattern is different, and complete quadrangle, nanometer sheet thickness can not have been kept to be about 3.5nm。
Embodiment 6
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.461g PbI2In adding the straight test tube of length, will Examination ferrule, adds 7.5ml HI solution to dissolve PbI by syringe2Powder, then added by syringe on the upper strata of solution Enter 15ml absolute methanol solutions as cushion, finally by syringe 0.3ml phenyl ethylamine solution is injected；
2) by Jing steps 1) reactant liquor that processes stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is separated out in cushion, is gradually increased to reaction later stage flat crystal.The flat crystal that will be separated out Take out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in toluene in the ratio of 1mg/ml, The ultrasound 30min under the ultrasonic power of 240W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
By (the C for preparing6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The micro- Electronic Speculum (AFM) of sub- power characterizes, and nanometer sheet pattern is different, and complete quadrangle, nanometer sheet thickness can not have been kept to be about 2.1nm。
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention.It is all the present invention spirit and Within principle, any modification, equivalent substitution and improvements made etc. should be included within the scope of the present invention.

Claims (6)

1. the liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet, it is characterised in that comprise the following steps：
1) in an inert atmosphere, metal halide powder is added in test tube, ferrule will be tried, by syringe into test tube Add halogen acids to dissolve above-mentioned powder, then absolute methanol solution is injected as cushion on the upper strata of solution, finally by injection Liquid organic amine needed for device injection reaction, described organic amine and the mol ratio of metal halide is 2:1；
2) by Jing steps 1) process reactant liquor stand at least 2 week, cushion separate out flat crystal, will separate out sheet Crystal takes out, after cleaning 2～3 times with absolute ether, vacuum drying；
3) flat crystal that vacuum drying is obtained is dispersed in low polarity stripper in the ratio of 1mg/ml, in gentle condition Under it is ultrasonically treated, you can obtain the two-dimentional perovskite nanometer sheet suspension of atomic-level thickness.
2. the liquid phase strip preparation method of atomic-level thickness according to claim 1 two dimension perovskite nanometer sheet, its feature It is that described metal halide is lead halide PbX2, halogen acids is HX, and wherein X is Br or I.
3. the liquid phase strip preparation method of atomic-level thickness according to claim 1 two dimension perovskite nanometer sheet, its feature It is that described low polarity stripper is toluene solution.
4. the liquid phase strip preparation method of atomic-level thickness according to claim 1 two dimension perovskite nanometer sheet, its feature It is that described gentle ultrasound condition is：Power is 60～240W, ultrasonic 5～30min of duration.
5. the liquid phase strip preparation method of atomic-level thickness according to claim 1 two dimension perovskite nanometer sheet, its feature It is that described inert atmosphere is realized that preparation process is carried out in glove box, and oxygen content, water content are equal in glove box by glove box Less than 0.5ppm.
6. the liquid phase strip preparation method of atomic-level thickness according to claim 1 two dimension perovskite nanometer sheet, its feature It is that described liquid organic amine is phenyl ethylamine, and molecular formula is C6H5C2H4NH3。
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Cited By (4)

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CN108300470A (en) * 2017-12-25 2018-07-20 华中科技大学 A kind of preparation method of quasi- low-dimensional bismuthino perovskite nano material
CN108409582A (en) * 2018-03-19 2018-08-17 西北大学 A kind of preparation method of perovskite thin film
CN108893114A (en) * 2018-06-25 2018-11-27 中山大学 A kind of unleaded halide perovskite quantum dot and preparation method thereof
CN116675608A (en) * 2023-05-31 2023-09-01 天津大学 Method for preparing blue perovskite quantum dots in situ by single crystal powder

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108300470A (en) * 2017-12-25 2018-07-20 华中科技大学 A kind of preparation method of quasi- low-dimensional bismuthino perovskite nano material
CN108300470B (en) * 2017-12-25 2019-12-20 华中科技大学 Preparation method of quasi-low-dimensional bismuth-based perovskite nano material
CN108409582A (en) * 2018-03-19 2018-08-17 西北大学 A kind of preparation method of perovskite thin film
CN108893114A (en) * 2018-06-25 2018-11-27 中山大学 A kind of unleaded halide perovskite quantum dot and preparation method thereof
CN108893114B (en) * 2018-06-25 2021-09-21 中山大学 Lead-free halide perovskite quantum dot and preparation method thereof
CN116675608A (en) * 2023-05-31 2023-09-01 天津大学 Method for preparing blue perovskite quantum dots in situ by single crystal powder
CN116675608B (en) * 2023-05-31 2024-03-08 天津大学 Method for preparing blue perovskite quantum dots in situ by single crystal powder

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