CN116462225A - CsPbBr 3 Preparation method of nano-sheet - Google Patents

CsPbBr 3 Preparation method of nano-sheet Download PDF

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CN116462225A
CN116462225A CN202310482589.2A CN202310482589A CN116462225A CN 116462225 A CN116462225 A CN 116462225A CN 202310482589 A CN202310482589 A CN 202310482589A CN 116462225 A CN116462225 A CN 116462225A
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cspbbr
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sheet
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高妍
宋济安
吕薇
江泽龙
胡桃
门凡钞
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Wuyi University
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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Abstract

The invention belongs to the technical field of nanometer luminescent material synthesis, and particularly discloses CsPbBr 3 A preparation method of a nano-sheet. The preparation method comprises the following steps: pouring CsBr powder into HBr solution, and obtaining Cs precursor solution after ultrasonic dispersion; pbBr is prepared 2 Pouring the powder into an organic solvent, ultrasonically dissolving, injecting a surface end-capping ligand, and stirring to obtain PbBr 2 A precursor solution; surface capping ligands include oleylamine and tri-n-octylphosphine; pbBr is prepared 2 Injecting the precursor solution into the cyclohexane under stirring; then injecting a Cs precursor solution for reaction; refillAcetone is added to obtain CsPbBr 3 A crude solution of nanoplatelets; centrifuging the crude solution, discarding supernatant, and injecting into toluene. CsPbBr synthesized by the invention 3 The fluorescence quantum yield of the nano-sheet is high and can reach 87.1%; the half-width is narrow, only 13.2nm, and has good optical performance.

Description

CsPbBr 3 Preparation method of nano-sheet
Technical Field
The invention belongs to the technical field of nanometer luminescent material synthesis, and in particular relates to CsPbBr 3 A preparation method of a nano-sheet.
Background
All-inorganic metal halide perovskites have received great attention for their excellent optoelectronic properties such as long carrier lifetime, high defect tolerance, band gap tunability, and narrow emission linewidth. Materials that achieve perovskite blue light emission are typically: csPbCl 3 Quantum dot, csPbClxBr 3-x Quantum dot (0)<x<3) However, the low luminous efficiency and the easy separation limit the development of the light-emitting diode; low-dimensional CsPbBr 3 Nanomaterials (e.g. zero-dimensional CsPbBr 3 Quantum dot and one-dimensional CsPbBr 3 Nanocrystalline) can also achieve perovskite blue light emission, but all face synthesis difficulties and stability problems.
Two-dimensional CsPbBr 3 Nanoplatelets having large exciton binding energy, short fluorescence lifetime are considered ideal perovskite blue light emitting materials. The surface end-capping ligand used in the synthesis process is adsorbed on the surface of the nano material to isolate external moisture and oxygen, so that the influence of the surface end-capping ligand on the inorganic layer structure is reduced, and the surface end-capping ligand is an indispensable step in the perovskite nano crystal synthesis process. However, csPbBr is easily caused by ligand shedding 3 The luminous efficiency of the nano-sheet is reduced and the emission peak is red shifted.
Thus, selection of the appropriate surface capping ligand for synthesis of high quality CsPbBr 3 The nano-sheet has a critical effect.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems in the prior art described above. For this purpose, the invention provides a CsPbBr 3 Preparation method of nanosheets, which uses oleylamine and tri-n-octylphosphine as surface end-capping ligandsAcetone is used as demulsifier, HBr protonated oleylamine is adopted, and a microemulsion method is adopted to synthesize high-quality CsPbBr under the condition of room temperature 3 A nano-sheet.
To solve the above technical problems, a first aspect of the present invention provides a CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
pouring CsBr powder into HBr solution, and obtaining Cs precursor solution after ultrasonic dispersion;
PbBr is prepared 2 Pouring the powder into an organic solvent, ultrasonically dissolving, injecting a surface end-capping ligand, and stirring to obtain PbBr 2 A precursor solution; the surface capping ligands include oleylamine and tri-n-octylphosphine;
the PbBr is processed 2 Injecting the precursor solution into the cyclohexane under stirring; then injecting the Cs precursor solution for reaction; then acetone is injected to obtain CsPbBr 3 A crude solution of nanoplatelets;
centrifuging the crude solution, discarding supernatant, and injecting into toluene to obtain CsPbBr 3 A nano-sheet.
Specifically, the invention synthesizes the two-dimensional perovskite nano-sheet by adopting a microemulsion method under the room temperature condition, takes oleylamine and tri-n-octyl phosphine as surface end-capping ligands, takes acetone as demulsifier, and takes HBr protonated oleylamine to synthesize high-quality CsPbBr 3 A nano-sheet. Wherein: the surface end-capped ligand adopts a mixture of oleylamine and tri-n-octylphosphine, and at present, oleylamine and/or oleic acid are often used as the surface end-capped ligand in the synthesis process of the perovskite nano-sheet, but the oleic acid is easily desorbed from the surface of the nano-crystal so as to induce defect generation. The invention creatively introduces tri-n-octyl phosphine and utilizes the strong binding force of tri-n-octyl phosphine and the nano crystal surface to inhibit CsPbBr 3 Nanosheet surface atomic vibration and ligand desorption reduce defect generation, thereby improving CsPbBr 3 The synthesis quality of the nano-sheet.
CsPbBr of the present invention 3 In the preparation process of the nano-sheet, preparing corresponding precursor solution: pbBr is prepared 2 Dissolving in organic solvent, adding oleylamine and tri-n-octyl phosphine to obtain PbBr 2 Precursor solutionThe method comprises the steps of carrying out a first treatment on the surface of the CsBr is dissolved in HBr to obtain a Cs precursor solution; pbBr is then processed 2 Injecting the precursor solution into vigorously stirred cyclohexane, and then injecting the Cs precursor solution; finally adding acetone to induce CsPbBr 3 The nanoplatelets nucleate and grow.
As a further improvement of the above scheme, the volume ratio of the oleylamine to tri-n-octylphosphine is (2-10): 1.
preferably, the volume ratio of the oleylamine to the tri-n-octylphosphine is (3-6): 1.
as a further improvement of the above scheme, the concentration of the Cs precursor solution is 0.2-6mmol/mL.
Preferably, the concentration of the Cs precursor solution is 0.5-1.5mmol/mL.
As a further improvement of the above scheme, the PbBr 2 The concentration of the precursor solution is 0.1-2.5mmol/mL.
Preferably, the PbBr 2 The concentration of the precursor solution is 0.2-1.0mmol/mL.
As a further improvement of the above, the cyclohexane solution and the PbBr 2 The volume ratio of the precursor solution is (7.5-30): 1.
preferably, the cyclohexane solution and the PbBr 2 The volume ratio of the precursor solution is (12-18): 1.
as a further improvement of the above, the Cs precursor solution and the PbBr 2 The usage amount of the precursor solution is (0.1-1.4) according to the mol ratio of Cs to Pb: 1.
preferably, the Cs precursor solution and the PbBr 2 The usage amount of the precursor solution is (0.1-0.5) according to the mol ratio of Cs to Pb: 1.
as a further improvement of the above scheme, the volume ratio of the acetone to the cyclohexane is (0.1-0.4): 1.
preferably, the volume ratio of the acetone to the cyclohexane is (0.1-0.3): 1.
preferably, the organic solvent is selected from the group consisting of N, N-Dimethylformamide (DMF) and dimethylsulfoxide.
Preferably, the time of the ultrasonic dispersion is 20 to 30 minutes.
Preferably, the time of the ultrasonic dissolution is 20-35 minutes.
Preferably, the stirring speed is 900-1000 rpm.
Preferably, the reaction time is 30 to 40 seconds.
Preferably, the rotational speed of the centrifugation is 9000-10000 rpm, and the time of the centrifugation is 2-3 minutes.
Compared with the prior art, the technical scheme of the invention has at least the following technical effects or advantages:
(1) The invention takes oleylamine and tri-n-octyl phosphine as surface end-capping ligands, acetone as demulsifier, and HBr is used for protonating oleylamine to synthesize CsPbBr 3 A nano-sheet. Wherein: the surface end-capped ligand (oleylamine and tri-n-octylphosphine) has strong binding force with the surface of the nanocrystal, thus inhibiting CsPbBr 3 The atomic vibration and ligand desorption on the surface of the nano-sheet reduce the generation of defects. Synthesized CsPbBr 3 The fluorescence quantum yield of the nano-sheet is high and can reach 87.1%; the half-width is narrow, only 13.2nm, and has good optical performance.
(2) The invention synthesizes CsPbBr by adopting a microemulsion method at room temperature 3 The nano-sheet has short reaction period and low synthesis cost. And the prepared PbBr 2 The precursor can be stored for a long time without adding oleylamine and tri-n-octylphosphine surface end capping ligands.
Drawings
FIG. 1 is CsPbBr prepared in example 1 3 An emission and absorption spectrum of the nanoplatelets;
FIG. 2 is CsPbBr prepared in example 1 3 Fluorescence quantum yield map of nanoplatelets;
FIG. 3 is CsPbBr prepared in example 1 3 Transverse transmission electron microscopy of nanoplatelets;
FIG. 4 is CsPbBr prepared in example 1 3 Transmission electron microscopy of the lateral thickness of the nanoplatelets;
FIG. 5 is CsPbBr prepared in example 1 and comparative examples 1-2 3 Fluorescence spectrum of nanoplatelets.
Detailed Description
The present invention is described in detail below with reference to examples to facilitate understanding of the present invention by those skilled in the art. It is specifically pointed out that the examples are given solely for the purpose of illustration of the invention and are not to be construed as limiting the scope of the invention, since numerous insubstantial modifications and variations of the invention will be within the scope of the invention, as described above, will become apparent to those skilled in the art. Meanwhile, the raw materials mentioned below are not specified, and are all commercial products; the process steps or preparation methods not mentioned in detail are those known to the person skilled in the art.
Example 1
CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
(1) Pouring 0.5mmol of CsBr powder into 0.5mL of HBr solution (with the concentration of 40%), and ultrasonically dispersing until the solution is colorless and transparent to obtain Cs precursor solution;
(2) 0.25mmol of PbBr 2 The powder was poured into 0.5mL of DMF solution and sonicated until PbBr was reached 2 Completely dissolving; then 0.41mL of oleylamine and 0.09mL of tri-n-octylphosphine are injected and stirred continuously before use to obtain cloudy milky PbBr 2 A precursor solution;
(3) 3mL of cyclohexane was placed in a clear glass bottle and stirred at 900 rpm; then taking 0.2mL of PbBr prepared in the step (2) 2 The precursor solution is rapidly injected into the cyclohexane solution under stirring, and stirring is continued for 30 seconds;
(4) Injecting 27.5 mu L of the Cs precursor solution prepared in the step (1) into the step (3) under stirring, and reacting for 30 seconds; then 0.6mL of acetone is injected to promote CsPbBr 3 The nanosheets nucleate and grow, and the process is continuously stirred for 90 seconds to obtain CsPbBr 3 A crude solution of nanoplatelets;
(5) Centrifuging the crude solution obtained in the step (4) at 9000 rpm for 2 minutes, then pouring out the supernatant, and injecting 2mL of toluene to obtain CsPbBr of the embodiment 3 A nanosheet solution.
Example 2
CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
(1) Pouring 0.5mmol of CsBr powder into 0.5mL of HBr solution (with the concentration of 40%), and ultrasonically dispersing until the solution is colorless and transparent to obtain Cs precursor solution;
(2) 0.25mmol of PbBr 2 The powder was poured into 0.5mL of DMF solution and sonicated until PbBr was reached 2 Completely dissolving; then 0.41mL of oleylamine and 0.09mL of tri-n-octylphosphine are injected and stirred continuously before use to obtain cloudy milky PbBr 2 A precursor solution;
(3) 3mL of cyclohexane was placed in a clear glass bottle and stirred at 900 rpm; then taking 0.2mL of PbBr prepared in the step (2) 2 The precursor solution is rapidly injected into the cyclohexane solution under stirring, and stirring is continued for 30 seconds;
(4) Injecting 26 mu L of the Cs precursor solution prepared in the step (1) into the step (3) in stirring, and reacting for 30 seconds; then 0.6mL of acetone is injected to promote CsPbBr 3 The nanosheets nucleate and grow, and the process is continuously stirred for 90 seconds to obtain CsPbBr 3 A crude solution of nanoplatelets;
(5) Centrifuging the crude solution obtained in the step (4) at 9000 rpm for 2 minutes, then pouring out the supernatant, and injecting 2mL of toluene to obtain CsPbBr of the embodiment 3 A nanosheet solution.
Example 3
CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
(1) Pouring 0.5mmol of CsBr powder into 0.5mL of HBr solution (with the concentration of 40%), and ultrasonically dispersing until the solution is colorless and transparent to obtain Cs precursor solution;
(2) 0.25mmol of PbBr 2 The powder was poured into 0.5mL of DMF solution and sonicated until PbBr was reached 2 Completely dissolving; then 0.41mL of oleylamine and 0.09mL of tri-n-octylphosphine are injected and stirred continuously before use to obtain cloudy milky PbBr 2 A precursor solution;
(3) In a transparent glass3mL of cyclohexane is added into the glass bottle, and stirring is carried out at the speed of 900 revolutions per minute; then taking 0.2mL of PbBr prepared in the step (2) 2 The precursor solution is rapidly injected into the cyclohexane solution under stirring, and stirring is continued for 30 seconds;
(4) Injecting 28 mu L of the Cs precursor solution prepared in the step (1) into the step (3) in stirring, and reacting for 30 seconds; then 0.6mL of acetone is injected to promote CsPbBr 3 The nanosheets nucleate and grow, and the process is continuously stirred for 90 seconds to obtain CsPbBr 3 A crude solution of nanoplatelets;
(5) Centrifuging the crude solution obtained in the step (4) at 9000 rpm for 2 minutes, then pouring out the supernatant, and injecting 2mL of toluene to obtain CsPbBr of the embodiment 3 A nanosheet solution.
Comparative example 1
CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
(1) Pouring 0.5mmol of CsBr powder into 0.5mL of HBr solution (with the concentration of 40%), and ultrasonically dispersing until the solution is colorless and transparent to obtain Cs precursor solution;
(2) 0.25mmol of PbBr 2 The powder was poured into 0.5mL of DMF solution and sonicated until PbBr was reached 2 Completely dissolving; then 0.5mL of oleylamine is injected and stirred continuously before use to obtain turbid milky PbBr 2 A precursor solution;
(3) 3mL of cyclohexane was placed in a clear glass bottle and stirred at 900 rpm; then taking 0.2mL of PbBr prepared in the step (2) 2 The precursor solution is rapidly injected into the cyclohexane solution under stirring, and stirring is continued for 30 seconds;
(4) Injecting 27.5 mu L of the Cs precursor solution prepared in the step (1) into the step (3) under stirring, and reacting for 30 seconds; then 0.6mL of acetone is injected to promote CsPbBr 3 The nanosheets nucleate and grow, and the process is continuously stirred for 90 seconds to obtain CsPbBr 3 A crude solution of nanoplatelets;
(5) Centrifuging the crude solution obtained in the step (4) at 9000 rpm for 2 minutes, then pouring out the supernatant, and injecting 2mL of toluene to obtain CsPbBr of the comparative example 3 Nanometer scaleAnd (3) a tablet solution.
Comparative example 1 differs from example 1 only in that: comparative example 1 employs oleylamine as a surface capping ligand.
Comparative example 2
CsPbBr 3 The preparation method of the nano-sheet comprises the following steps:
(1) Pouring 0.5mmol of CsBr powder into 0.5mL of HBr solution (with the concentration of 40%), and ultrasonically dispersing until the solution is colorless and transparent to obtain Cs precursor solution;
(2) 0.25mmol of PbBr 2 The powder was poured into 0.5mL of DMF solution and sonicated until PbBr was reached 2 Completely dissolving; then 0.41mL of oleylamine and 0.09mL of oleic acid are injected and stirred continuously before use to obtain cloudy milky PbBr 2 A precursor solution;
(3) 3mL of cyclohexane was placed in a clear glass bottle and stirred at 900 rpm; then taking 0.2mL of PbBr prepared in the step (2) 2 The precursor solution is rapidly injected into the cyclohexane solution under stirring, and stirring is continued for 30 seconds;
(4) Injecting 27.5 mu L of the Cs precursor solution prepared in the step (1) into the step (3) under stirring, and reacting for 30 seconds; then 0.6mL of acetone is injected to promote CsPbBr 3 The nanosheets nucleate and grow, and the process is continuously stirred for 90 seconds to obtain CsPbBr 3 A crude solution of nanoplatelets;
(5) Centrifuging the crude solution obtained in the step (4) at 9000 rpm for 2 minutes, then pouring out the supernatant, and injecting 2mL of toluene to obtain CsPbBr of the comparative example 3 A nanosheet solution.
Comparative example 2 differs from example 1 only in that: comparative example 2 employs oleylamine and oleic acid as surface-capping ligands.
Performance testing
FIG. 1 is CsPbBr prepared in example 1 3 Emission and absorption spectra of nanoplatelets, wherein: the abscissa Wavelength represents Wavelength, the ordinate PL intensity represents light excitation intensity, and absorptance represents Absorbance. As can be seen from FIG. 1, the sample exhibited strong exciton absorption at about 456nm with tri-n-octylphosphine and oleylamine ligand modification, its emissionThe peak is at about 464nm and the corresponding full width at half maximum (FWHM) is 13.2nm.
FIG. 2 is CsPbBr prepared in example 1 3 Fluorescence quantum yield plot of nanoplatelets, wherein: the abscissa Wavelength represents Wavelength, the ordinate Intensity represents Intensity, and the specification in the figure represents Excitation. As can be seen from FIG. 2, csPbBr under tri-n-octylphosphine and oleylamine ligand modification 3 The fluorescence quantum yield (PLQY) of the nanoplatelets can reach 87.1%.
FIG. 3 is CsPbBr prepared in example 1 3 Transverse transmission electron microscopy of nanoplatelets demonstrating CsPbBr based on tri-n-octylphosphine and oleylamine ligand modification 3 The lateral dimension morphology of the nanoplatelets.
FIG. 4 is CsPbBr prepared in example 1 3 Transmission electron microscopy of the lateral thickness of nanoplatelets, showing CsPbBr based on tri-n-octylphosphine and oleylamine ligand modification 3 The lateral thickness of the nanoplatelets is only about 3nm, which is also CsPbBr 3 The nanoplatelets can achieve the cause of blue light emission.
FIG. 5 is CsPbBr prepared in example 1 and comparative examples 1-2 3 Fluorescence spectrum of nanoplatelets. From FIG. 5, it can be seen that the oleylamine alone modifies CsPbBr 3 Nanosheets (comparative example 1) or CsPbBr co-modified with oleylamine and oleic acid 3 Nanosheets (comparative example 2) both have lower fluorescence emission intensities than CsPbBr modified with oleylamine and tri-n-octylphosphine ligands 3 Nanoplatelets (example 1).
Example 2 and example 3 preparation of CsPbBr 3 The performance of the nanoplatelets is similar to that of example 1 and will not be described in detail herein.
It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the inventive concept. Accordingly, it is intended that all such modifications as would be within the scope of this invention be included within the scope of this invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent modifications are intended to fall within the scope of the present invention.

Claims (10)

1. CsPbBr 3 The preparation method of the nano-sheet is characterized by comprising the following steps:
pouring CsBr powder into HBr solution, and obtaining Cs precursor solution after ultrasonic dispersion;
PbBr is prepared 2 Pouring the powder into an organic solvent, ultrasonically dissolving, injecting a surface end-capping ligand, and stirring to obtain PbBr 2 A precursor solution; the surface capping ligands include oleylamine and tri-n-octylphosphine;
the PbBr is processed 2 Injecting the precursor solution into the cyclohexane under stirring; then injecting the Cs precursor solution for reaction; then acetone is injected to obtain CsPbBr 3 A crude solution of nanoplatelets;
centrifuging the crude solution, discarding supernatant, and injecting into toluene to obtain CsPbBr 3 A nano-sheet.
2. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the volume ratio of the oleylamine to the tri-n-octyl phosphine is (2-10): 1.
3. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the concentration of the Cs precursor solution is 0.2-6mmol/mL.
4. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the PbBr 2 The concentration of the precursor solution is 0.1-2.5mmol/mL.
5. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the cyclohexane solution and the PbBr 2 The volume ratio of the precursor solution is (7.5-30): 1.
6. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the CsPrecursor solution and the PbBr 2 The usage amount of the precursor solution is (0.1-1.4) according to the mol ratio of Cs to Pb: 1.
7. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the volume ratio of the acetone to the cyclohexane is (0.1-0.4): 1.
8. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the organic solvent is selected from N, N-dimethylformamide or dimethyl sulfoxide.
9. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the ultrasonic dispersion time is 20-30 minutes; the ultrasonic dissolution time is 20-35 minutes.
10. CsPbBr according to claim 1 3 The preparation method of the nano-sheet is characterized in that the stirring rotating speed is 900-1000 rpm; the reaction time is 30-40s; the rotational speed of the centrifugation is 9000-10000 revolutions per minute, and the time of the centrifugation is 2-3 minutes.
CN202310482589.2A 2023-04-28 2023-04-28 CsPbBr 3 Preparation method of nano-sheet Pending CN116462225A (en)

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Cited By (1)

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CN116970392A (en) * 2023-08-01 2023-10-31 上海工程技术大学 In-situ ligand modified CsPbBr 3 Preparation method and application of nanosheet material

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CN113684025A (en) * 2021-09-02 2021-11-23 张家松 Synthesis method of halide perovskite type nanocrystal quantum dot
CN114864835A (en) * 2022-04-19 2022-08-05 北京科技大学 Blue light perovskite quantum dot film, electroluminescent diode and preparation
CN115536059A (en) * 2022-10-26 2022-12-30 五邑大学 CsPbBr 3 Nanosheet and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN113684025A (en) * 2021-09-02 2021-11-23 张家松 Synthesis method of halide perovskite type nanocrystal quantum dot
CN114864835A (en) * 2022-04-19 2022-08-05 北京科技大学 Blue light perovskite quantum dot film, electroluminescent diode and preparation
CN115536059A (en) * 2022-10-26 2022-12-30 五邑大学 CsPbBr 3 Nanosheet and preparation method and application thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116970392A (en) * 2023-08-01 2023-10-31 上海工程技术大学 In-situ ligand modified CsPbBr 3 Preparation method and application of nanosheet material

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