CN106631816B - A kind of liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet - Google Patents

A kind of liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet Download PDF

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CN106631816B
CN106631816B CN201611206573.5A CN201611206573A CN106631816B CN 106631816 B CN106631816 B CN 106631816B CN 201611206573 A CN201611206573 A CN 201611206573A CN 106631816 B CN106631816 B CN 106631816B
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CN106631816A (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 kind of preparation methods of atomic-level thickness two dimension perovskite nanometer sheet, using liquid phase stripping method, two-dimentional perovskite block materials are first specifically prepared with layer solwution method, ultrasonic wave added stripping method is recycled, the nanometer sheet at atomic-level thickness is removed using the lower stripper of polarity and by two-dimentional perovskite block materials liquid phase under mild stripping conditions.Preparation method of the present invention is convenient and easy, and the two-dimentional perovskite ultrathin nanometer piece thickness of acquisition can maintain single layer between a few atomic 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, nanometer sheet obtained has single 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, Quantum Well 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 pass through it is certain Method is removed at when the ultra-thin materials of single layer or several atomic layer level thickness, and jumbo increased specific surface area not only increases material The physics and chemism for expecting surface also affect the two-dimentional wave function caused by 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 increasingly maturation of lift-off technology, there are many two at present Dimension material be successfully able to be separated into independent nano flake, as graphene (Graphene), transient metal sulfide (TMDs), Metal-organic framework material (MOFs) etc., they have all shown excellent physicochemical characteristics.
Researcher has carried out various methods and has attempted the stripping of two-dimentional block materials into the nano flake of atomic-level thickness, liquid phase Stripping is one of main method.Liquid phase stripping be in certain medium by ultrasonic means by two-dimensional ultrathin nanometer sheet from Be stripped out in respective masses material, to obtain two-dimensional ultrathin nanometer sheet colloidal solution method.It is (molten by stripping media Agent and auxiliary reagent) screening can effectively improve the charge stripping efficiency of nanometer sheet.Liquid phase stripping largely, can be obtained uniformly because of it It obtains two-dimensional ultrathin nanometer sheet and is widely studied, nowadays have become a kind of more mature stripping means.Currently, 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 have excellent photoelectric properties, and become nowadays burning the hotest photovoltaic material.It is short Five, between 6 years, the photoelectric conversion efficiency of the solar cell based on this perovskite-like is promoted from 3.8% to 22.1%.
Ideal perovskite structure is cubic crystal structure, by total vertex MX6Octahedron is constituted, it is in three-dimensional unlimited extension Reticular structure is formed, the smaller atom of radius or molecule A are located in octahedral interstice.For three-dimensional organic and inorganic perovskite material Material, M are typically a kind of divalent metal atom, and X indicates that halogen atom, wherein metal cation M are located at octahedra center, and smaller Organic molecule A (be usually methylamine) be filled in the dodecahedron gap that six adjacent octahedrons surround, general structure is AMX3.And when organic cation molecular chain length is larger, so that it may be respectively formed A according to organic cation valence state2MX4(A is+1 Valence) or AMX4The two-dimensional layer perovskite-like structure of (A is+divalent) two kinds of forms, wherein A cation are generally RNH3 +Or NH3RNH3 2+(R is alkyl or aryl radical).Studies have shown that for the case where R is alkyl, organic moiety C atom numbers It will appear perovskite when more than 3 from three-dimensional to two-dimensional structure to be changed, and when R is aryl radical, organic moiety master Chain C atom numbers 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 organic cation and inorganic halides anion Mode combines, 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 binding force, but currently, there is no liquid phase stripping method prepare atomic-level thickness two-dimentional perovskite ultrathin nanometer piece report.
Invention content
The object of the present invention is to provide a kind of sides preparing atomic-level thickness two dimension perovskite nanometer sheet based on liquid phase stripping Method, this method are to be combined the architectural characteristic of atomic-level thickness two-dimensional material with the excellent photoelectric properties of perovskite material, profit With liquid phase lift-off technology, realizes the ultra-thin preparation of two-dimentional perovskite, obtain the two-dimentional perovskite nanometer sheet of atomic-level thickness.
The preparation method of the atomic-level thickness two dimension perovskite nanometer sheet of the present invention, using 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 to examination Halogen acids is added in pipe and dissolves above-mentioned powder, then in the upper layer of solution injection absolute methanol solution as buffer layer, finally by The molar ratio of liquid organic amine needed for syringe injection reaction, the organic amine and metal halide is 2:1；Halogen acids and Methanol excess；
2) reaction solution handled through step 1) is stood at least two week, flat crystal is precipitated in buffer layer, by precipitation Flat crystal takes out, after cleaning 2~3 times with anhydrous ether, vacuum drying；
3) flat crystal that vacuum drying obtains is dispersed in the ratio of 1mg/ml in low polarity stripper, mild Under the conditions of be 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 HX, wherein X are Br or I.
Above-mentioned liquid organic amine is phenyl ethylamine, molecular formula C6H5C2H4NH3。
The big flat crystal of above-mentioned precipitation is two-dimentional perovskite block stratified material, and molecular formula is (C6H5C2H4)2PbX4, Middle X is Br or I.Existing document shows (C6H5C2H4NH3)2PbX4Single layer atomic thickness is in 1.75nm or so.
Method used in the method for the present invention mainly contains two steps.The first step is that layer solwution method prepares two-dimentional perovskite block Body material.Second step is the liquid phase stripping process of block materials, is 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 obtains can maintain single layer to several Between a atomic layer.
In reaction process of the present invention, stripper uses toluene solution, is the strong ion characteristic due to perovskite material, stripping The polarity of liquid is no more than ether.
It is the mechanical fragility due to two-dimentional perovskite material using mild ultrasound condition in reaction process of the present invention, Violent ultrasound condition easily causes the organic fraction of two-dimentional perovskite to be broken.The temperate condition typically refer to power 60~ 240W, ultrasonic 5~30min of duration.
The method that ultrasonic wave added stripping prepares two-dimentional perovskite nanometer sheet requires external environment, equipment etc. 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 implementation mode
Embodiment 1
1) it is respectively less than in the glove box of 0.5ppm in oxygen content, water content, weighs 0.367g PbBr2Long straight test tube is added In, ferrule will be tried, 7.5ml HBr solution, which is added, by syringe dissolves PbBr2Powder, then pass through note on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in emitter, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous 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.
(the C that will be prepared6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) characterizes, and nanometer sheet pattern keeps complete quadrangle, and nanometer sheet thickness is 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 PbBr2Long straight test tube is added In, ferrule will be tried, 7.5ml HBr solution, which is added, by syringe dissolves PbBr2Powder, then pass through note on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in emitter, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous 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.
(the C that will be prepared6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) characterizes, and nanometer sheet pattern is different, can not keep the complete quadrangle, nanometer sheet thickness 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 PbBr2Long straight test tube is added In, ferrule will be tried, 7.5ml HBr solution, which is added, by syringe dissolves PbBr2Powder, then pass through note on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in emitter, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of white plates are had during reaction (C6H5C2H4NH3)2PbBr4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous 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 outstanding Supernatant liquid.
(the C that will be prepared6H5C2H4NH3)2PbBr4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, it is carried out Atomic force microscopy Electronic Speculum (AFM) characterizes, and nanometer sheet pattern is different, can not keep the complete quadrangle, nanometer sheet thickness 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 PbI2Long straight test tube is added In, ferrule will be tried, 7.5ml HI solution, which is added, by syringe dissolves PbI2Powder, then pass through injection on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in device, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in the ratio of 1mg/ml in toluene, The ultrasound 5min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
(the C that will be prepared6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The sub- micro- Electronic Speculum of power (AFM) characterization, nanometer sheet pattern keep complete quadrangle, and nanometer sheet thickness is 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 PbI2Long straight test tube is added In, ferrule will be tried, 7.5ml HI solution, which is added, by syringe dissolves PbI2Powder, then pass through injection on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in device, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in the ratio of 1mg/ml in toluene, The ultrasound 30min under the ultrasonic power of 60W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
(the C that will be prepared6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The sub- micro- Electronic Speculum of power (AFM) characterization, nanometer sheet pattern is different, can not keep the complete quadrangle, nanometer sheet thickness 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 PbI2Long straight test tube is added In, ferrule will be tried, 7.5ml HI solution, which is added, by syringe dissolves PbI2Powder, then pass through injection on the upper layer of solution 15ml absolute methanol solutions are added as buffer layer in device, inject 0.3ml phenyl ethylamine solution finally by syringe；
2) reaction solution that will be handled through step 1) stood for 2 week, and a large amount of orange-yellow sheets are had during reaction (C6H5C2H4NH3)2PbI4Crystal is precipitated in buffer layer, gradually increases to reaction later stage flat crystal.By the flat crystal of precipitation It takes out, after cleaning 2~3 times with anhydrous ether, vacuum drying；
3) (the C for obtaining vacuum drying6H5C2H4NH3)2PbI4Flat crystal is dispersed in the ratio of 1mg/ml in toluene, The ultrasound 30min under the ultrasonic power of 240W the, you can obtain (C of atomic-level thickness6H5C2H4NH3)2PbI4Nanometer sheet suspension.
(the C that will be prepared6H5C2H4NH3)2PbI4Nanometer sheet hanging drop is coated in SiO2On/Si substrates, original is carried out to it The sub- micro- Electronic Speculum of power (AFM) characterization, nanometer sheet pattern is different, can not keep the complete quadrangle, nanometer sheet thickness to be about 2.1nm。
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention.It is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (2)

1. the liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet, which is characterized in that include 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 Halogen acids is added and dissolves above-mentioned powder, then absolute methanol solution is injected as buffer layer, finally by injection on the upper layer of solution The molar ratio of liquid organic amine needed for device injection reaction, the organic amine and metal halide is 2:1；The metal halogen Compound is lead halide PbX2, halogen acids HX, wherein X are Br or I, and the liquid organic amine is phenyl ethylamine, and molecular formula is C6H5C2H4NH2；
2）It will be through step 1）The reaction solution of processing stands at least two week, flat crystal is precipitated in buffer layer, by the sheet of precipitation Crystal takes out, after cleaning 2 ~ 3 times with anhydrous ether, vacuum drying；
3）The flat crystal that vacuum drying obtains is dispersed in the ratio of 1mg/ml in low polarity stripper, in mild condition Lower supersound process, you can obtain the two-dimentional perovskite nanometer sheet suspension of atomic-level thickness；The low polarity stripper is first Benzole soln, the mild ultrasound condition are：Power is 60 ~ 240 W, 5 ~ 30 min of ultrasonic duration.
2. the liquid phase strip preparation method of atomic-level thickness two dimension perovskite nanometer sheet according to claim 1, feature It is that the inert atmosphere is realized by glove box, preparation process carries out in glove box, and oxygen content, water content are equal in glove box Less than 0.5 ppm.
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