CN115595149A - Preparation method of quantum dots with light-emitting life of ms grade - Google Patents

Preparation method of quantum dots with light-emitting life of ms grade Download PDF

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CN115595149A
CN115595149A CN202110771397.4A CN202110771397A CN115595149A CN 115595149 A CN115595149 A CN 115595149A CN 202110771397 A CN202110771397 A CN 202110771397A CN 115595149 A CN115595149 A CN 115595149A
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mapbi
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CN115595149B (en
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金盛烨
尹子夕
孙祺
冷静
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Dalian Institute of Chemical Physics of CAS
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Abstract

The invention provides a preparation method of quantum dots with apparent life of ms, which comprises the following steps: 1) Taking appropriate amount of lead acetate and Zn (NO) 3 ) 2 ·6H 2 Dissolving O in water; 2) Dissolving proper amount of dimethyl imidazole and isophthalic acid in water to obtain clear solution; 3) Dropwise adding the solution obtained in the step 1) into the solution obtained in the step 2) under vigorous stirring to obtain white precipitate, performing centrifugal separation, and performing vacuum drying for later use; 4) Dissolving appropriate amount of iodomethylamine crystal in anhydrous ethanol to obtain colorlessA clear solution; 5) Soaking a proper amount of the powder obtained in the step 3) in the solution obtained in the step 4), centrifuging, washing with absolute ethyl alcohol, and drying in vacuum. The MOF material Y346 has a lifetime of triplet on the order of seconds and can emit phosphorescence through Y346 triplet itself and MAPbI 3 The energy transfer between the quantum dots can greatly improve the apparent service life of the quantum dots and improve the stability of the quantum dots. The adjusting method has the advantages of simplicity and easiness in operation, easiness in obtaining raw materials, low equipment requirement and the like, and is expected to produce good environmental, social and economic effects.

Description

Preparation method of quantum dots with light-emitting life of ms grade
Technical Field
The invention relates to a preparation method of quantum dots with the luminescent life of ms grade.
Technical Field
The metal halide perovskite has the advantages of adjustable optical performance, simple and variable preparation method, easily obtained raw materials and the like, thereby obtaining wide attention in the photoelectric and photovoltaic fields, being regarded as a photoelectric and photovoltaic material with very promising prospect, and showing excellent performance in the fields of solar cells, luminescent devices, detectors and the like. The perovskite quantum dots have strong quantum confinement effect, so that most excitons can emit photons in a fluorescence radiation recombination mode after absorbing excited photons, have high fluorescence quantum yield, and are commonly used for light-emitting devices such as LEDs and the like. However, the conventional thermal injection method is not only complicated in experimental operation, but also the prepared metal halide perovskite quantum dot is short in fluorescence lifetime and poor in light stability, and further application of the metal halide perovskite quantum dot is limited.
In the invention, the MOF material Y346 used is simple to prepare, has good stability and has good tolerance to external conditions such as illumination, water vapor and the like. The study finds that the energy transfer from the singlet state to the triplet state exists in Y346, phosphorescence is generated after photoexcitation, the phosphorescence lifetime can reach the second level, the phosphorescence emission wavelength almost covers the whole visible wavelength band, and the wavelength band with the strongest phosphorescence intensity is just the same as MAPbI 3 The absorption peaks of the quantum dots are close in position. Thus, MAPbI was grown in situ in Y346 using a co-precipitation method 3 The quantum dots can not only improve the stability of the perovskite quantum dots, but also utilize Y346 to MAPbI 3 The energy transfer of quantum dots can obviously improve MAPbI 3 The apparent life of the quantum dots provides a new idea for modulating the fluorescence performance and improving the stability of the perovskite quantum dots. To our knowledge, no report on the preparation method of the quantum dot with the luminescent lifetime of ms is available, so the development of the quantum dotThe preparation method of the quantum dots with the luminescent life of ms level has important significance.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of quantum dots with the luminescent life of ms grade aiming at the prior art, which comprises the following steps: preparing Pb-doped Y346 by a coprecipitation method, soaking a certain amount of Pb-doped Y346 in an ethanol solution of iodomethylamine (MAI), centrifugally separating, washing and drying to obtain MAPbI with high stability and ms-grade apparent luminescence life 3 And (4) quantum dots.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the quantum dots with the luminescent life of ms grade is characterized by comprising the following steps in sequence:
1) Collecting 0.5690-2.845g of lead acetate and 1.1457-5.7285g of Zn (NO) 3 ) 2 ·6H 2 Dissolving O in deionized water;
2) Dissolving 0.492-2.46g of dimethylimidazole and 0.498-2.49g of isophthalic acid in deionized water to obtain a clear solution;
3) Dropwise adding the solution obtained in the step 1) into the solution obtained in the step 2) under vigorous stirring to obtain white precipitate, performing centrifugal separation, and performing vacuum drying for later use;
4) Dissolving a proper amount of iodomethylamine crystals in absolute ethyl alcohol to obtain a colorless transparent solution;
5) Soaking a proper amount of the powder obtained in the step 3) in the solution obtained in the step 4), centrifuging, washing with absolute ethyl alcohol, and drying in vacuum.
According to the scheme, the using amount of the deionized water in the step 1) is 3-10ml;
according to the scheme, the using amount of the deionized water in the step 2) is 3-10ml;
according to the scheme, the centrifugal separation rotating speed in the step 3) is 5000-8000rpm, and the centrifugal time is 5-10 min;
according to the scheme, the vacuum drying temperature in the step 3) is 40-60 ℃;
according to the scheme, the dosage of the MAI in the step 4) is 0.564-1.692g, and the dosage of the absolute ethyl alcohol is 5-10ml;
according to the scheme, the centrifugal separation rotating speed in the step 5) is 5000-8000rpm;
according to the scheme, the centrifugation time in the step 5) is 5min-10min;
according to the scheme, the soaking time in the step 5) is 5-15min;
according to the scheme, the vacuum drying temperature in the step 5) is 40-60 ℃.
The MOF material Y346 has a triplet state with the lifetime reaching the second order and can emit phosphorescence, and the invention provides that MAPbI is grown in situ in the Y346 3 Quantum dots using Y346 triplet to MAPbI 3 The energy transfer of the quantum dots modulates the luminescence property of the quantum dots, so that the apparent life of the quantum dots can be greatly prolonged, and the stability of the quantum dots is improved; make MAPbI 3 The apparent luminescence lifetime of quantum dots is increased to the order of milliseconds and has good stability.
MAPbI under 375nm ultraviolet excitation, with increasing irradiation time 3 The fluorescence emission spectrum of the quantum dots is gradually red-shifted and then the region is stable; the phosphorescence lifetime can reach millisecond order, and the stability is more stable than that of pure MAPbI prepared by a solution method 3 The quantum dots are increased remarkably.
The invention has the beneficial effects that: the invention utilizes Y346 to prepare MAPbI with apparent luminescence life millisecond level 3 The method for preparing the quantum dots has the advantages of simple and quick operation, simple device, easily obtained raw materials, low equipment requirement, easy mass production and the like, and is simple, economic and easy to prepare MAPbI with the apparent life of millisecond grade 3 The method of quantum dots is expected to produce good social and economic effects.
Drawings
FIG. 1 shows MAPbI in example 1 3 A transmission electron microscope photograph of @ Y346;
FIG. 2 shows MAPbI in example 1 3 Fluorescence emission spectra of @ Y346;
FIG. 3 shows MAPbI in example 1 3 Phosphorescence decay curves for @ Y346 quantum dots;
FIG. 4 shows MAPbI in example 1 3 The curve of fluorescence intensity with time @ Y346;
FIG. 5 is pure MAPbI 3 The change curve of the fluorescence intensity of the quantum dots along with time;
Detailed Description
The present invention will be described in further detail with reference to examples, but the present invention is not limited to these descriptions.
The prepared quantum dot luminescent property is characterized by fluorescence spectrum and dynamics. The experimental procedure was as follows: fluorescence spectra were collected with a spectrometer (SpectraPro-2300 i, acton Research Co., USA) using a 375nm laser (PDL 800-B, picoQuant, germany) as the excitation light source. Fluorescence lifetime was tested by a time-dependent single photon counting (TCSPC) system built in the laboratory itself.
Example 1:
1) 0.5690g of lead acetate and 1.1457g of Zn (NO) are taken 3 ) 2 ·6H 2 Dissolving O in 3ml of deionized water;
2) Dissolving 0.492g of dimethyl imidazole and 0.498g of isophthalic acid in 7ml of deionized water to obtain a clear solution;
3) Dropwise adding the solution obtained in the step 1) into the solution obtained in the step 2) under stirring to obtain a white precipitate, centrifuging at 5000rpm for 10min to separate a solid, and drying in vacuum at 40 ℃ for later use;
4) Dissolving 0.564g of iodomethylamine crystals in 5ml of absolute ethanol to obtain a colorless transparent solution;
5) Soaking 0.08g of the powder obtained in the step 3) in the solution obtained in the step 4), centrifuging at 5000rpm for 10min to separate solid, washing with absolute ethyl alcohol, and vacuum drying at 40 ℃ to obtain MAPbI 3 Sample @ Y346.
FIG. 1 is MAPbI 3 The @ Y346 sample was photographed using transmission electron microscopy, the inset is MAPbI 3 The particle size distribution diagram of the quantum dots is obtained, and MAPbI is seen from the diagram 3 Indeed, it exists within the Y346 skeleton, and the quantum dot transmission picture is circular, with a particle size range of 2nm to 5.5 nm, and an average particle size of about 3.48 nm. (MA is an abbreviation of methylamino)
Example 2:
to explore Y346 vs MAPbI 3 Influence of fluorescence characteristics of quantum dots, we used fluorescence microscope, waveLaser excitation at 375nm for the MAPbI prepared in example 1 3 Fluorescence spectroscopy and lifetime testing was performed @ Y346:
FIG. 2 is MAPbI 3 Fluorescence emission Spectroscopy of @ Y346 in order to excite Y346 and MAPbI simultaneously 3 The quantum dot uses 375nm laser as an excitation light source, spectrum collection is carried out while laser irradiation is carried out, Y346 can be seen to present a wide emission spectrum with the wavelength ranging from 450 nanometers to 600 nanometers, MAPbI 3 The fluorescence emission spectrum center of the quantum dot is 772nm, the wavelength range of the spectrum is 640nm to 800nm, and a certain confinement effect is presented, which is caused by that the size of the particle reaches the nanometer level, the electronic energy level near the Fermi level is split into discrete energy levels by a continuum state, so that the MAPbI with a certain quantum confinement effect is really grown in situ in Y346 3 And (4) quantum dots.
FIG. 3 is MAPbI 3 The phosphorescence attenuation curve of @ Y346 quantum point, the excitation wavelength adopts 375 nanometers, the single photon detector is utilized to collect dynamics, and MAPbI can be seen 3 MAPbI in @ Y346 3 The phosphorescence lifetime of (2) can reach 3ms magnitude.
Example 3:
to prepare the MAPbI obtained in example 1 3 The illumination stability of @ Y346 is characterized, spectra of different illumination time are collected under 375nm laser continuous illumination, and fluorescence intensity of quantum dot fluorescence emission wavelength range (640 nm-800 nm) at different moments is compared.
FIG. 4 shows MAPbI in example 1 3 Curve of fluorescence intensity over time for fluorescence emission spectra of quantum dots of @ Y346. Under the irradiation of an ultraviolet lamp at 375nm, MAPbI 3 The luminous intensity of the quantum dot in @ Y346 was increased with the increase of irradiation time in the first 200min, and after 200min, the fluorescence intensity was gradually decreased with the irradiation time, but the fluorescence was not completely disappeared after 700min of irradiation, showing good stability.
Example 4:
as a control, we prepared pure MAPbI 3 Quantum dot:
1) 0.0159g of iodomethylamine is taken and0.0461g PbI 2 dissolved in 1ml DMF;
2) Adding 200 mu L of oleic acid and 10 mu L of n-butylamine into the solution obtained in the step 1), and heating and stirring at 30 ℃ for 30min;
3) Adding 10 mu L of the solution obtained in the step 2) into 4ml of toluene under stirring to obtain a precipitate;
4) Centrifuging at 5000rpm for 5min, and separating supernatant to obtain precipitate;
5) Adding 200 mu L of oleic acid and 20 mu L of oleylamine into 20ml of n-hexane to obtain a solution a;
6) Adding the 2ml solution o into the precipitate obtained by centrifugation, performing ultrasonic dispersion, then performing centrifugation at 5000rpm for 5min, and taking the supernatant to obtain a quantum dot solution.
Example 5:
is the same as pure MAPbI 3 Comparison of the stability of the quantum dots, we prepared pure MAPbI 3 Quantum dots were subjected to stability testing, and FIG. 5 shows pure MAPbI prepared in example 4 under different irradiation times 3 The curve of the change of the fluorescence intensity of the quantum dots along with the time shows that the fluorescence almost completely disappears after 8min, which indicates that MAPbI prepared in example 1 3 @ Y346 pure MAPbI prepared as in example 4 3 The stability of the quantum dots is greatly improved.

Claims (5)

1. A preparation method of quantum dots with light-emitting life of ms grade is characterized by comprising the following steps:
1) Collecting 0.5690-2.845g of lead acetate and 1.1457-5.7285g of Zn (NO) 3 ) 2 ·6H 2 Dissolving O in 3-10ml deionized water;
2) Dissolving 0.492-2.46g of dimethylimidazole and 0.498-2.49g of isophthalic acid in 5-10ml of deionized water to obtain a clear solution;
3) Dropwise adding the solution obtained in the step 1) into the solution obtained in the step 2) under stirring to obtain a white precipitate, performing centrifugal separation, and performing vacuum drying on the solid for later use;
4) Dissolving 0.564-1.692g of iodomethylamine crystals in 5-10ml of absolute ethanol to obtain colorless transparent solution;
5) Soaking 0.02g-0.1g of the solid powder obtained in the step 3) in the solution obtained in the step 4), centrifuging, washing the solid with absolute ethyl alcohol, and drying in vacuum.
2. The method for preparing quantum dots with light-emitting life of ms grade according to claim 1, wherein the method comprises the following steps: the centrifugal separation rotating speed in the step 3) is 5000-8000rpm, and the centrifugal time is 5-10 min.
3. The method for preparing quantum dots with the luminescent lifetime of ms grade according to claim 1, wherein the method comprises the following steps: the vacuum drying temperature in the step 3) is 40-60 ℃.
4. The method for preparing quantum dots with the luminescent lifetime of ms grade according to claim 1, wherein the method comprises the following steps: the centrifugal separation rotating speed in the step 5) is 5000-8000rpm, and the centrifugal time is 5-10 min.
5. The method for preparing quantum dots with the luminescent lifetime of ms grade according to claim 1, wherein the method comprises the following steps: in the step 5), the soaking time is 5-15min, and the vacuum drying temperature is 40-60 ℃.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109762178A (en) * 2019-02-11 2019-05-17 洛阳师范学院 A kind of metal-organic framework materials, metal-organic framework materials of rhodamine B-sensitized and its preparation method and application
CN110041915A (en) * 2019-04-24 2019-07-23 深圳大学 The preparation method of perovskite quantum dot and metal organic frame composite luminescent material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109762178A (en) * 2019-02-11 2019-05-17 洛阳师范学院 A kind of metal-organic framework materials, metal-organic framework materials of rhodamine B-sensitized and its preparation method and application
CN110041915A (en) * 2019-04-24 2019-07-23 深圳大学 The preparation method of perovskite quantum dot and metal organic frame composite luminescent material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
SUN QI: "Encapsulation of CH3NH3PbBr3 Perovskite Quantum Dots in MOF-5 Microcrystals as a Stable Platform for Temperature and Aqueous Heavy Metal Ion Detection", 《JOURNAL OF PHYSICAL CHEMISTRY LETTERS》, vol. 11, no. 21 *

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