CN110144210A - A kind of preparation method of bromide perovskite quantum dot - Google Patents
A kind of preparation method of bromide perovskite quantum dot Download PDFInfo
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- CN110144210A CN110144210A CN201910541106.5A CN201910541106A CN110144210A CN 110144210 A CN110144210 A CN 110144210A CN 201910541106 A CN201910541106 A CN 201910541106A CN 110144210 A CN110144210 A CN 110144210A
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- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
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Abstract
The invention discloses a kind of preparation methods of bromide perovskite quantum dot, include the following steps: that methylamine or carbonamidine ammonium bromide, metal bromide, n-octyl amine and oleic acid are dissolved in N by (1), in dinethylformamide, stirring obtains perovskite quantum dot precursor liquid；(2) it takes dodecylphosphoric acid to be dissolved in weak polar solvent, obtains the weak polar solvent solution of dodecylphosphoric acid；(3) the perovskite quantum dot precursor liquid of step (1) is added in toluene solution, is sufficiently stirred, obtains the perovskite quantum dot solution of clear yellow green；(4) by the perovskite quantum dot solution centrifugal purification of the yellow green of step (3), the weak polar solvent solution of the dodecylphosphoric acid of step (2) is added, is sufficiently stirred, fully reacting, the perovskite quantum dot solution being passivated.The advantages that stability that bromide perovskite quantum dot prepared by the present invention has is good, fluorescence intensity is high big with the size of quantum dot.
Description
Technical field
The present invention relates to the preparation method of quantum dot light emitting material, in particular to a kind of system of bromide perovskite quantum dot
Preparation Method.
Background technique
Perovskite quantum dot shows that lighting area has good application development in light emitting diode, quantum dot TV etc..Calcium
Titanium ore quantum dot is a kind of semiconductor material of solution processable, has significant photoelectronic property, such as high-luminous-efficiency, extremely narrow
Luminescence spectrum, very wide colour gamut and the features such as easier band gap adjustability, the luminescent color of quantum dot can simply lead to
Size and halogen atom ratio are crossed to adjust, to obtain shining for visible-range, high color purity and wide colour gamut are expected to make
Its candidate for becoming next generation display.
Although perovskite quantum dot shows excellent luminescent properties, in actual production process, still have
Problem limits their large-scale application, and maximum problem is unstability of the perovskite quantum dot to environmental factor,
Under the conditions ofs ultraviolet light, humidity, oxygen, solvent, temperature etc. rapid aggregate and precipitate, even decompose.With hybrid inorganic-organic calcium titanium
For mine quantum dot, due to the weak binding characteristic between the oleic acid and octylame on Colloidal Quantum Dots surface, in the mistake of centrifugal purification
The oleic acid of quantum dot surface and octylame ligand are easily separated from plane of crystal in journey, unstable so as to cause the quantum dot property of synthesis
It is fixed, and then influence its function and use.
Summary of the invention
A kind of goal of the invention: the bromine that it is an object of the present invention to provide stability is good, the high size with quantum dot of fluorescence intensity is big
The preparation method of compound perovskite quantum dot.
Technical solution: the present invention provides a kind of preparation method of bromide perovskite quantum dot, includes the following steps:
(1) methylamine or carbonamidine ammonium bromide, metal bromide, n-octyl amine and oleic acid are dissolved in n,N-Dimethylformamide
In, stirring obtains perovskite quantum dot precursor liquid；
(2) it takes dodecylphosphoric acid to be dissolved in weak polar solvent, obtains the weak polar solvent solution of dodecylphosphoric acid；
(3) the perovskite quantum dot precursor liquid of step (1) is added in toluene solution, is sufficiently stirred, obtains clear Huang
The perovskite quantum dot solution of green；
(4) by the perovskite quantum dot solution centrifugal purification of the yellow green of step (3), the dodecyl of step (2) is added
The weak polar solvent solution of phosphoric acid, is sufficiently stirred, fully reacting, the perovskite quantum dot solution being passivated,
Above-mentioned each reaction carries out under room temperature environment.
It further, include 12 carbon atoms in the long-chain of the dodecylphosphoric acid.The weak polar solvent be toluene,
Chlorobenzene, n-hexane or acetonitrile.The metal bromide is lead bromide, stannic bromide or bromination germanium.The methylamine or carbonamidine ammonium bromide
Mass ratio with metal bromide is 1.2: 1.In 530nm or so, half-peak breadth is less than the luminous peak position of the perovskite quantum dot
25nm。
Technical method of the invention uses the strong phase of dodecylphosphoric acid and the lead ion in lead bromide perovskite quantum dot
Part is replaced the oleic acid and octylame ligand of quantum dot surface by interaction, is passivated the defect of quantum dot surface, is improved quantum dot
Stability.Using dodecylphosphoric acid as passivator, the addition of dodecylphosphoric acid on the one hand can be with bromide perovskite
Metal ion in quantum dot combines, so that part replaces the oleic acid and octylame ligand of quantum dot surface, is passivated quantum dot surface
Defect, improve the stability of quantum dot；On the other hand quantum dot surface Br ion can also be made to pass through hydrogen bond or electrostatic phase interaction
With in conjunction with alkyl amine cation, in addition, strong in conjunction with nucleation and quantum can also be accelerated between this ligand and lead ion
The growth of point.
The utility model has the advantages that the stability for the bromide perovskite quantum dot that the present invention is prepared is good, fluorescence intensity Gao Yiliang
The size of son point is big；Equipment needed for the method for the present invention is simple to operation, low in cost, is not necessarily to high temperature, can synthesize at room temperature,
It is easy to spread；The narrow quanta point material of high brightness of the invention, glow peak has preferable application prospect in display, lighting area.
Detailed description of the invention
Fig. 1 is the PL spectrum of the present embodiment perovskite quantum dot solution；
Fig. 2 is the XRD spectrum of the present embodiment perovskite quantum dot solution；
Fig. 3 is that the TEM of the present embodiment perovskite quantum dot solution (sample A) schemes；
Fig. 4 is that the TEM of the present embodiment perovskite quantum dot solution (sample C) schemes.
Specific embodiment
The preparation method of the bromide perovskite quantum dot of the present embodiment, includes the following steps:
(1) synthesis of perovskite quantum dot
By the CH (NH of 0.48mmol2)2(lead bromide) PbBr of Br (carbonamidine ammonium bromide), 0.40mmol2, 500 μ L oleic acid
It is dissolved in the n,N-Dimethylformamide (DMF) of 4mL with the n-octyl amine of 30 μ L, stirs 30 minutes, form transparent perovskite
Quantum dot precursor liquid.Then 250 μ L perovskite quantum dot precursor liquids are instilled in the toluene solution for the 10mL being vigorously stirred.This
When, toluene solution immediately becomes yellow-green soln after mixing.All reactions carry out under 23.5 DEG C of room temperature of environmental condition.
(2) passivation of perovskite quantum dot
The dodecylphosphoric acid of 0.05g is dissolved in the toluene solution of 5mL, the toluene solution of dodecylphosphoric acid is obtained.
Then perovskite quantum dot solution centrifugal purification, 6000rpm is arranged in centrifuge speed.After being centrifuged 5min, collected with bottle
Perovskite quantum dot solution, the toluene solution of dodecylphosphoric acid and toluene (constant volume use) are 2000 according to volume ratio by clear liquid
: 0: 600,2000: 400: 200,2000: 500: 100,2000: 600: 0, the calcium titanium that sample ID is A, B, C and D is prepared respectively
Mine quantum dot solution, and be stirred at room temperature, the perovskite quantum dot solution after forming passivation.
Fig. 1 is fluorescent emission (PL) spectral line of perovskite quantum dot solution prepared by the present embodiment 1；Using of the invention
Perovskite quantum dot prepared by the method for perovskite quantum dot is prepared, quantum-dot structure is not changed.With do not use dodecane
Base phosphoric acid processing perovskite quantum dot compare, the PL intensity that the perovskite quantum dot of dodecylphosphoric acid is added be remarkably reinforced and
There is red shift, illustrates that dodecylphosphoric acid can improve the fluorescence intensity of perovskite quantum dot well and increase the ruler of quantum dot
It is very little.
Fig. 2 is the XRD spectral line of perovskite quantum dot solution prepared by embodiment 1.Perovskite quantum is prepared using the present invention
Perovskite quantum dot prepared by the method for point, does not change the lattice structure of quantum dot.With the addition of dodecylphosphoric acid,
Perovskite quantum dot is obviously increased at 15 ° with 30 ° of peak intensity, illustrates that its crystallinity enhances；Peak width narrows simultaneously, illustrates addition ten
Perovskite quantum dot after Acidic phosphates becomes large-sized, this coincide with PL spectra shift, TEM test result.
Fig. 3 is the TEM picture of perovskite quantum dot solution (sample A) prepared by embodiment 1.Use system of the present invention
The toluene solvant of perovskite quantum dot prepared by the method for standby perovskite quantum dot has dispersibility well, perovskite quantum
The structure cubic of point.
Fig. 4 is the TEM picture of perovskite quantum dot solution (sample C) prepared by embodiment 1.Use system of the present invention
The structure of perovskite quantum dot prepared by the method for standby perovskite quantum dot changes without the addition because of dodecylphosphoric acid
Become, only becomes large-sized.
Claims (6)
1. a kind of preparation method of bromide perovskite quantum dot, characterized by the following steps:
(1) methylamine or carbonamidine ammonium bromide, metal bromide, n-octyl amine and oleic acid are dissolved in n,N-Dimethylformamide, are stirred
It mixes, obtains perovskite quantum dot precursor liquid；
(2) it takes dodecylphosphoric acid to be dissolved in weak polar solvent, obtains the weak polar solvent solution of dodecylphosphoric acid；
(3) the perovskite quantum dot precursor liquid of step (1) is added in toluene solution, is sufficiently stirred, obtains clear yellow green
Perovskite quantum dot solution；
(4) by the perovskite quantum dot solution centrifugal purification of the yellow green of step (3), the dodecylphosphoric acid of step (2) is added
Weak polar solvent solution, be sufficiently stirred, fully reacting, the perovskite quantum dot solution being passivated,
Above-mentioned each reaction carries out under room temperature environment.
2. the preparation method of bromide perovskite quantum dot according to claim 1, it is characterised in that: the dodecyl
It include 12 carbon atoms in the long-chain of phosphoric acid.
3. the preparation method of bromide perovskite quantum dot according to claim 1, it is characterised in that: the low pole is molten
Agent is toluene, chlorobenzene, n-hexane or acetonitrile.
4. the preparation method of bromide perovskite quantum dot according to claim 1, it is characterised in that: the metal bromide
Object is lead bromide, stannic bromide or bromination germanium.
5. the preparation method of bromide perovskite quantum dot according to claim 1, it is characterised in that: the methylamine or first
The mass ratio of amidine ammonium bromide and metal bromide is 1.2: 1.
6. the preparation method of bromide perovskite quantum dot according to claim 1, it is characterised in that: the perovskite amount
For the luminous peak position of son point in 530nm or so, half-peak breadth is less than 25nm.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349437A (en) * | 2020-04-21 | 2020-06-30 | 陕西科技大学 | Perovskite quantum dot based on castor oil as green solvent and preparation method thereof |
| CN111718709A (en) * | 2020-07-01 | 2020-09-29 | 合肥福纳科技有限公司 | Post-processing method and preparation method of quantum dots, prepared quantum dots and application |
| CN112574738A (en) * | 2020-12-17 | 2021-03-30 | 扬州大学 | Preparation method for improving stability of perovskite quantum dots |
| CN112694418A (en) * | 2021-02-01 | 2021-04-23 | 西北大学 | Preparation method of formamidine bromo-perovskite quantum dots with controllable sizes |
| CN113736448A (en) * | 2021-08-28 | 2021-12-03 | 浙江大学温州研究院 | Modified halogen perovskite quantum dot and preparation method thereof |
| WO2023087449A1 (en) * | 2021-11-17 | 2023-05-25 | 中国科学院深圳先进技术研究院 | Manganese-doped organic perovskite cluster material and preparation method therefor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298978A (en) * | 2017-07-03 | 2017-10-27 | 中山大学 | A kind of preparation method of the leaded halide perovskite quantum dot fluorescence powder of full-inorganic |
| CN108258157A (en) * | 2018-01-22 | 2018-07-06 | 苏州大学 | perovskite quantum dot and its synthetic method |
| CN109652060A (en) * | 2019-01-17 | 2019-04-19 | 南京邮电大学 | A kind of synthesis preparation method of organic polymer perovskite quantum dot and its application |
-
2019
- 2019-06-21 CN CN201910541106.5A patent/CN110144210A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298978A (en) * | 2017-07-03 | 2017-10-27 | 中山大学 | A kind of preparation method of the leaded halide perovskite quantum dot fluorescence powder of full-inorganic |
| CN108258157A (en) * | 2018-01-22 | 2018-07-06 | 苏州大学 | perovskite quantum dot and its synthetic method |
| CN109652060A (en) * | 2019-01-17 | 2019-04-19 | 南京邮电大学 | A kind of synthesis preparation method of organic polymer perovskite quantum dot and its application |
Non-Patent Citations (1)
| Title |
|---|
| TONGTONG XUAN ET AL.，: "Highly stable CsPbBr3 quantum dots coated with alkyl phosphate for white light-emitting diodes及其Supporting Information", 《NANOSCALE》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111349437A (en) * | 2020-04-21 | 2020-06-30 | 陕西科技大学 | Perovskite quantum dot based on castor oil as green solvent and preparation method thereof |
| CN111718709A (en) * | 2020-07-01 | 2020-09-29 | 合肥福纳科技有限公司 | Post-processing method and preparation method of quantum dots, prepared quantum dots and application |
| CN112574738A (en) * | 2020-12-17 | 2021-03-30 | 扬州大学 | Preparation method for improving stability of perovskite quantum dots |
| CN112574738B (en) * | 2020-12-17 | 2022-10-28 | 扬州大学 | Preparation method for improving stability of perovskite quantum dots |
| CN112694418A (en) * | 2021-02-01 | 2021-04-23 | 西北大学 | Preparation method of formamidine bromo-perovskite quantum dots with controllable sizes |
| CN112694418B (en) * | 2021-02-01 | 2022-05-17 | 西北大学 | Preparation method of formamidine bromo-perovskite quantum dots with controllable sizes |
| CN113736448A (en) * | 2021-08-28 | 2021-12-03 | 浙江大学温州研究院 | Modified halogen perovskite quantum dot and preparation method thereof |
| WO2023087449A1 (en) * | 2021-11-17 | 2023-05-25 | 中国科学院深圳先进技术研究院 | Manganese-doped organic perovskite cluster material and preparation method therefor |
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Application publication date: 20190820 |