CN111233030B - Perovskite CsPbBr3Preparation method of nanosheet - Google Patents
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Abstract
The invention relates to perovskite CsPbBr3A preparation method of a nano-sheet belongs to the technical field of inorganic nano-material preparation. The invention adopts a synthesis method of hot injection and uses 10-undecaynoic acid as a surface ligand to synthesize CsPbBr3Quantum dots are dispersed in cyclohexane. Then the sample is taken under an ultraviolet lamp for irradiation, and the CsPbBr with regular shape and appearance is successfully prepared3Nanosheets. The method has simple steps and strong repeatability, and is used for preparing the perovskite CsPbBr with uniform appearance3Nanoplatelets are a viable approach. CsPbBr prepared under irradiation of ultraviolet lamp3The nanosheets showed significant green emission and a lifetime ratio CsPbBr3The quantum dots are obviously increased, and the excellent optical properties enable the quantum dots to have wide application in the fields of flat panel display and the like.
Description
Technical Field
The invention relates to perovskite CsPbBr3A preparation method of a nano-sheet belongs to the technical field of inorganic nano-material preparation.
Background
In 2009, organic-inorganic perovskites were first reported to be applied in the solar field, and the perovskite has become a star material in many fields due to the excellent performance of continuous excavation. 2015, SwitzerlandThe Maksym professor topic group reports inorganic perovskite quantum dots CsPbX for the first time3(Protesescu，L.；Yakunin，S.；Bodnarchuk，M.I.；Krieg，F.；Caputo，R.；Hendon，C. H.；Yang，R.X.；Walsh，A.；Kovalenko，M.V.，Nanocrystals of Cesium Lead Halide Perovskites(CsPbX3X ═ Cl, Br, and I): novel Optoelectronic Materials displaying Bright Emission with Wide Color gamut nano Lett 2015, 15, 3692-6), the quantum yield is up to 90%, the luminescent Color is adjustable in the whole visible light range, and the luminescent material has great potential in the luminescent field. From this point, CsPbX3Research on application of perovskite materials to the field of photoelectricity enters a rapid development stage. This rate of development is quite dramatic compared to the development of organic fluorescent dyes and conventional quantum dot light emitting diodes for over 20 years. The perovskite quantum dot material becomes a research hotspot in the field of new generation light-emitting diodes due to the high color purity, high external quantum efficiency, and the relatively simple and good-repeatability solution preparation method.
However, CsPbX3The grain size, dimension, morphology and the like of the perovskite material have great influence on the photoelectric properties of the material. When the crystal grain of the material is increased from the nano scale to the micron scale, the band gap energy of the material is reduced, the radiation recombination efficiency coefficient is increased, the service life of the material is prolonged, and the material can easily realize higher photoelectric performance; liberato Manna et al CsPbBr3The perovskite quantum dots are assembled into a two-dimensional nano sheet structure, so that the luminous color of the material is changed. Meanwhile, the prepared nano-sheet structure has narrower half-peak width and stronger exciton absorption (Akkerman, Q.A.; Motti, S.G.; Kandada, A.R.S.; Mosconi, E.; D' Innoceonzo, V.; Bertoni, G.; Marras, S.; Kaminoo, B.A.; Miranda, L.; De Angelis, F.; Petrozza, A.; Prato, M.; Manna, L., Solution Synthesis to colloid center line fiber nanoparticles Peroplatel with single layer-Level thin contact roll.J. Am Chem Soc 2016, 138, 1010); also, it has been shown that CsPbX3The perovskite is prepared into a two-dimensional structure, and the energy conversion efficiency is improved by 13% while the stability is improved (Ma, C.Q.; Shen,d; ng, t.w.; lo, m.f.; lee, C.S., 2D Perovskits with Short Interlayer Distance for High-Performance Solar Cell application. adv Mater 2018, 30, 1800710); CsPbX made by self-assembly method, for example, Gabrile rain oa3Nanocrystals, normally synthesized CsPbX3CsPbX synthesized by self-assembly method with nano crystal phase comparison3Nanocrystals have superior fluorescence properties (Raino, G.; Becker, M.A.; Bodnarchuk, M.1.; Mahrt, R.F.; Kovalenko, M.V.; Stoferle, T., Superfluorescence from lead halide above quartz crystal dot superior. Nature 2018, 563, 671 675). For the above reasons, by developing CsPbX3The research work in the aspect of perovskite self-assembly adjusts the size, dimension and morphology of the material, and has important scientific significance and application value.
Disclosure of Invention
The invention aims to provide perovskite CsPbBr3Preparation method of nanosheet and perovskite CsPbBr prepared by adopting preparation method3The nano-sheet has uniform morphology and good dispersibility, and a product obtained by reaction is of a cubic phase crystal structure and has good luminescence performance.
The invention provides perovskite CsPbBr3The preparation method of the nanosheet comprises the following steps:
(1) adding 0.1-0.3g of lead bromide into 7.5-20mL of octadecene;
(2) adding 0.03-0.09g of 10-undecaynoic acid into the mixed solution, and stirring;
(3) adding 1.5-4.5mL of oleylamine into the mixed solution, and stirring;
(4) heating the mixed solution to 125 ℃ of 120-;
(5) adding 0.35-0.70g of cesium carbonate into 10-20mL of octadecene;
(6) then adding 0.75-1.5mL of oleic acid into the mixed solution;
(7) stirring the mixed solution, heating to 150-170 ℃ until the solid in the mixed solution is completely dissolved, and naming the mixed solution as solution 2;
(8) taking 1-3mL of solution 2, quickly injecting the solution into the solution 1, and then quickly cooling the solution to room temperature by using an ice water bath;
(9) then adding absolute ethyl alcohol into the solution, centrifugally separating the product, wherein the rotation speed of a centrifugal machine is 10000-12000 r/min, and then adding cyclohexane to obtain CsPbBr3A quantum dot solution.
(10) The obtained CsPbBr3Putting the quantum dot solution into a glass vial, placing the vial in a spectral chamber with constant temperature, and irradiating with ultraviolet lamps with wavelengths of 254nm and 365nm for 6-8 hours in a dark box type ultraviolet analyzer to obtain CsPbBr3Nanosheets.
The invention has the beneficial effects that: CsPbBr prepared by thermal injection method3The quantum dots are uniform in size, and then the quantum dots can be assembled into CsPbBr with uniform appearance under the irradiation of ultraviolet light3Nanosheets. The obtained CsPbBr3The nano-sheets are pure cubic phases. CsPbBr prepared by assay3Quantum dots and CsPbBr3The emission spectrum of the nano sheet is that the green luminescence color purity of the obtained nano sheet is higher. CsPbBr can be clearly seen by naked eyes3Quantum dots and CsPbBr3The nanosheets differ significantly in color. The method is also suitable for other perovskites CsPbX3Preparation of (X ═ Cl, I) nanosheets.
Description of the drawings:
FIG. 1 perovskite CsPbBr prepared in example 1 of the present invention3Quantum dots (a) and perovskite CsPbBr3XRD spectrogram of the nano sheet (b).
FIG. 2A perovskite CsPbBr prepared in example 1 of the present invention3SEM photograph of nanoplatelets. The length of the nanoplatelets is about 500 nm.
FIG. 3A perovskite CsPbBr prepared in example 2 of the present invention3SEM photograph of nanoplatelets. The length of the nanoplatelets is about 250 nm.
FIG. 4 perovskite CsPbBr prepared in example 3 of the present invention3SEM photograph of nanoplatelets. The length of the nanoplatelets is about 1 μm.
FIG. 5 perovskite CsPbBr3Quantum dots and calciumTitanium ore CsPbBr3Emission spectra of the nanoplatelets. Compared with quantum dots, the luminescent color of the nano-sheet has purer green luminescence.
Detailed Description
Example 1
(1) 0.2g of lead bromide was added to 15mL of octadecene;
(2) adding 0.06g of 10-undecycolic acid into the mixed solution, and stirring;
(3) adding 3.0mL of oleylamine into the mixed solution, and stirring;
(4) heating the mixed solution, keeping the temperature, and then increasing the temperature to obtain a solution 1;
(5) 0.0735g of cesium carbonate was added to 20mL of octadecene;
(6) then adding 1.5mL of oleic acid into the mixed solution;
(7) stirring the mixed solution, and then heating until the solid in the mixed solution is completely dissolved, wherein the mixed solution is named as solution 2;
(8) taking 2mL of solution 2, quickly injecting the solution into the solution 1, and then quickly cooling the solution to room temperature by using an ice water bath;
(9) adding anhydrous ethanol into the solution, centrifuging to separate the product, and adding cyclohexane to obtain CsPbBr3A quantum dot solution.
(10) The obtained CsPbBr3Putting the quantum dot solution into a glass vial, taking a spectrum chamber with constant temperature, and illuminating for 6 hours in a dark box type ultraviolet analyzer by using an ultraviolet lamp with 365nm wavelength to obtain CsPbBr3Nanosheets.
FIG. 2 shows CsPbBr obtained by the reaction3SEM pictures of nanoplatelets.
Example 2
(1) 0.1g of lead bromide was added to 7.5mL of octadecene;
(2) adding 0.03g of 10-undecycolic acid into the mixed solution, and stirring;
(3) adding 1.5mL of oleylamine into the mixed solution, and stirring;
(4) heating the mixed solution, keeping the temperature, and then increasing the temperature to obtain a solution 1;
(5) 0.035g cesium carbonate was added to 10mL octadecene;
(6) then adding 0.75mL of oleic acid into the mixed solution;
(7) stirring the mixed solution, and then heating until the solid in the mixed solution is completely dissolved, wherein the mixed solution is named as solution 2;
(8) taking 1mL of solution 2, quickly injecting the solution into the solution 1, and then quickly cooling the solution to room temperature by using an ice water bath;
(9) adding anhydrous ethanol into the solution, centrifuging to separate the product, and adding cyclohexane to obtain CsPbBr3A quantum dot solution.
(10) The obtained CsPbBr3Putting the quantum dot solution into a glass vial, placing the vial in a spectral chamber with constant temperature, and illuminating with ultraviolet lamps with 254nm and 365nm wavelengths for 8 hours in a dark box type ultraviolet analyzer to obtain CsPbBr3Nanosheets.
FIG. 3 shows CsPbBr obtained by the reaction3SEM pictures of nanoplatelets.
Example 3
(1) Adding 0.3g of lead bromide to 20mL of octadecene;
(2) adding 0.09g of 10-undecycic acid into the mixed solution, and stirring;
(3) adding 4.5mL of oleylamine into the mixed solution, and stirring;
(4) heating the mixed solution, keeping the temperature, and then increasing the temperature to obtain a solution 1;
(5) 0.07g cesium carbonate was added to 20mL octadecene;
(6) then adding 2.25mL of oleic acid into the mixed solution;
(7) stirring the mixed solution, and then heating until the solid in the mixed solution is completely dissolved, wherein the mixed solution is named as solution 2;
(8) taking 3mL of the solution 2, quickly injecting the solution into the solution 1, and then quickly cooling the solution to room temperature by using an ice water bath;
(9) adding anhydrous ethanol into the solution, centrifuging to separate the product, and adding cyclohexane to obtain CsPbBr3A quantum dot solution.
(10) The obtained CsPbBr3Putting the quantum dot solution into a glass vial, placing the vial in a spectral chamber with constant temperature, and illuminating with an ultraviolet lamp with a wavelength of 254nm for 8 hours in a dark box type ultraviolet analyzer to obtain CsPbBr3Nanosheets.
FIG. 4 shows CsPbBr obtained by the reaction3SEM pictures of nanoplatelets.
Claims (7)
1. Perovskite CsPbBr3The preparation method of the nanosheet comprises the following steps:
(1) adding 0.1-0.3g of lead bromide into 7.5-20mL of octadecene;
(2) adding 0.03-0.09g of 10-undecaynoic acid into the mixed solution obtained in the step (1), and stirring;
(3) adding 1.5-4.5mL of oleylamine into the mixed solution obtained in the step (2), and stirring;
(4) heating the mixed solution, keeping the temperature, and then increasing the temperature to obtain a solution 1;
(5) adding 0.35-0.70g of cesium carbonate into 10-20mL of octadecene;
(6) then adding 0.75-1.5mL of oleic acid into the mixed solution obtained in the step (5);
(7) stirring the mixed solution obtained in the step (6), and then heating until the solid in the mixed solution is completely dissolved, wherein the name of the mixed solution is solution 2;
(8) taking 1-3mL of solution 2, quickly injecting the solution into the solution 1, and then quickly cooling the solution to room temperature by using an ice water bath;
(9) adding absolute ethyl alcohol into the solution obtained in the step (8), centrifugally separating the product, and adding cyclohexane to obtain CsPbBr3A quantum dot solution;
(10) the obtained CsPbBr3Putting the quantum dot solution into a glass vial, holding in a constant-temperature spectral chamber, and placing in a dark box
In an ultraviolet analyzer, an ultraviolet lamp is used for illumination to obtain CsPbBr3Nanosheets; the UV lamps have wavelengths of 254nm and 365 nm.
2. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: step (4)
The heating temperature in (1) is 120-125 ℃.
3. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: step (4)
The temperature holding time in (1) is 30 to 40 minutes.
4. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: step (4)
The temperature in (1) is raised to 130-135 ℃.
5. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: step (7)
To 150-.
6. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: step (9)
The rotational speed of the centrifuge in (1) is 10000-12000 revolutions per minute.
7. The perovskite CsPbBr of claim 13The preparation method of the nano-sheet is characterized by comprising the following steps: the illumination time in the step (10) is 6-8 h.
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