CN110003900A - A kind of high quantum production rate zero dimension perovskite structure pure phase Cs4PbBr6Material and synthetic method - Google Patents
A kind of high quantum production rate zero dimension perovskite structure pure phase Cs4PbBr6Material and synthetic method Download PDFInfo
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Abstract
The invention discloses a kind of high quantum production rate zero dimension perovskite structure pure phase Cs4PbBr6Material and synthetic method.The present invention assists reprecipitation method using simple ligand, by changing long short hydrocarbon organic ligand, and changes the ratio of organic ligand, fluorescence quantum yield is obtained under room temperature environment higher than 95%, half-peak breadth about 20nm, the 520nm green light of illuminant colour purity is high.Band gap is adjusted in addition, also the methods of exchanging with halide anion by changing different injection forerunner amounts, obtains the fluorescence spectrum of 450-630nm.The green light sample that the method obtains has good stability, and blue light, red light fluorescent powder is combined to be combined into white LED lamp.The present invention has broad application prospects in fields such as LED, FPD, solar batteries.
Description
Technical field
The present invention relates to a kind of high quantum production rate zero dimension perovskite structure pure phase Cs4PbBr6Material and synthetic method, belong to
Semiconductor nano material, technical field of photoelectric material preparation.
Background technique
Halide perovskite (ABX3) material of rising in recent years has excellent luminescence generated by light and electroluminescence characters,
Good application prospect is presented in fields such as solar battery, photodetector, LED light, displays；Research team both domestic and external
Also perovskite research ranks competitively be joined.However, with the further intensification of research, the problem of many its development and applications of restriction
Also it comes one after another.What is stood in the breach is stability；Based on this, extensive pass of the perovskite material of different phase structures by people
Note, and study its influence to optical property1,2.Especially zero dimension perovskite is because it is kept completely separate octahedron in lattice
[PbX6]4-Structure and have excellent stability3.Therefore, high PLQY high volume production pure phase zero dimension perovskite material is seemed
It is particularly important.
Bibliography.
(1) Wang, K. H.; Wu, L.; Li, L.; Yao, H. B.; Qian, H. S.; Yu, S. H.
Large-Scale Synthesis of Highly Luminescent Perovskite-Related CsPb2Br5
Nanoplatelets and Their Fast Anion Exchange. Angew. Chem., Int. Ed. 2016, 55, 8328−8332.
(2) Aharon, S.; Etgar, L. Two Dimensional Organometal Halide Perovskite
Nanorods with Tunable Optical Properties. Nano Lett. 2016, 16, 3230−3235.
(3) Chen, Y.; Zhou, Y.; Zhao, Q.; Zhang, J.; Ma, J.; Xuan, T.; Guo, S.;
Yong, Z.; Wang, J.; Kuroiwa, Y.; Moriyoshi, C.; Sun, Hong-Tao. Cs4PbBr6/
CsPbBr3 Perovskite Composites with Near-Unity Luminescence Quantum Yield:
Large-Scale Synthesis, Luminescence and Formation Mechanism, and White Light-
Emitting Diode Application. ACS Appl. Mater. Interfaces, 2018, 10, 15905。
Summary of the invention
The purpose of the present invention is to provide a kind of simple room temperatures to synthesize high quantum production rate pure phase zero dimension perovskite material, leads to
It crosses and changes long short hydrocarbon organic ligand, and change the ratio of organic ligand, obtain PLQY and be up to 95.1%, half-peak breadth about 20nm
520nm green light.
The present invention can be achieved through the following technical solutions, and steps are as follows.
Step 1, by metal halide salt BX2It is dissolved in dimethylformamide (DMF) with AX, ultrasound makes it completely dissolved.
Step 2, organic ligand is added in the DMF solution for the metal halide salt that step 1 obtains, is obtained after mixing
Reaction precursor liquid solution.
Step 3, reaction precursor liquid solution is added dropwise in anti-solvent, being stirred at room temperature makes fully reacting, is finally centrifuged, purifies
Obtain colloidal solution.
Step 4, by Cs4PbBr6Colloidal solution obtains the Cs of different band gap by anion metathesis4PbCl6With
Cs4PbI6Isocolloid solution.
Step 1, in 4, metal halide salt BX2For lead bromide (PbBr2), lead iodide (PbI2) or lead chloride (PbCl2),
AX is cesium bromide (CsBr).
Preferably, in step 2, the organic ligand is the mixture of oleic acid and lauryl amine, and volume ratio is 5:1 ~ 15:1.
Preferably, in step 2, the DMF solution of the metal halide salt and the volume ratio of organic ligand mixture are 5:1
~10:1。
Preferably, in step 3, the reaction dissolvent is ethyl acetate；Mixing speed is 1000r/min；Ambient temperature
It is 25 ~ 30 DEG C.
In reaction system, in reaction system, the molar ratio of metallic element Pb and Cs are 1:1 ~ 1:4.
Compared with prior art, the present invention has following remarkable result: preparation method of the invention can be by simple
Change presoma infusion volume, obtains the colloidal solution material at different luminescence generated by light peaks.Raw material needed for entire reaction are simple, instead
Short between seasonable, easy to operate, reaction condition is mild, reproducible, and product production rate is high, is conducive to produce in batches.
Detailed description of the invention.
Fig. 1 is pure phase perovskite Cs prepared by the embodiment of the present invention 14PbBr6TEM figure.
Fig. 2 is pure phase perovskite Cs prepared by the embodiment of the present invention 14PbBr6XRD diagram.
Fig. 3 is pure phase perovskite Cs prepared by the embodiment of the present invention 14PbBr6Optical property figure.
Fig. 4 is pure phase perovskite Cs prepared by the embodiment of the present invention 14PbBr6The LED of composition.
Fig. 5 is the pure phase perovskite Cs of 2-8 of embodiment of the present invention preparation4PbBr6Luminous spectrum.
Fig. 6 is pure phase perovskite Cs prepared by the embodiment of the present invention 1,33 and 344PbX6Sample and luminous spectrum.
Specific embodiment.
It elaborates below to the embodiment of the present invention.
A kind of high quantum production rate blue light perovskite Colloidal Quantum Dots material and synthetic method, first by metal halide salt BX2
It is dissolved in DMF with AX, and organic ligand is added, be then added dropwise to mixed liquor dropwise in the reaction dissolvent in stirring energetically,
Last BX2 and AX forms blue light perovskite Colloidal Quantum Dots material under the action of organic ligand.
Embodiment 1.
Step 1, the ethyl acetate that 10mL is added in the boiling flask of 20mL under room temperature, open magnetic agitation, stirring speed
Degree is 1000r/min, and stirring carries out in air, is not necessarily to inert gas shielding.
Step 2, by metal halide salt PbBr21:1 is dissolved completely in 5mlDMF in molar ratio with CsBr, and ultrasound makes metal
Halide salt is completely dissolved.
Step 3, into the DMF solution of metal halide salt, addition 0.5 ~ 1mL oleic acid, 25 ~ 200 μ l lauryl amines are matched as organic
Solution is uniformly mixed by body.
The mixed liquor that step 3 prepares is rapidly injected in ethyl acetate, obtained reaction by step 4 with volume ratio 1:100
Product removes bulky grain by 3000r/min centrifugal treating 5min, then precipitating dispersion is centrifuged in 12000r/min in hexane
5min is handled to get colloidal solution is arrived.
Zero dimension perovskite colloid pattern made from the present embodiment as shown in Figure 1, component and phase structure as shown in Fig. 2, its light
It learns performance and sees Fig. 3, emission wavelength 520nm, absorb band edge 515nm, volume production 95.1%.And blue light, red light fluorescent powder is combined to combine
At white LED lamp, shown in Fig. 4.
Embodiment 2.
Similar to Example 1, difference is in step 1, and the ethyl acetate of 1mL, step are added in the boiling flask of 20mL
In rapid 4,10 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions are consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 3.
Similar to Example 2, difference is in step 4,20 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions
It is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 4.
Similar to Example 2, difference is in step 4,30 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions
It is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 5.
Similar to Example 2, difference is in step 4,40 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions
It is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 6.
Similar to Example 2, difference is in step 4,50 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions
It is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 7.
Similar to Example 2, difference is in step 4,75 μ l of forerunner is added dropwise in ethyl acetate dropwise, other conditions
It is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 8.
Similar to Example 2, difference is in step 4, and 100 μ l of forerunner is added dropwise in ethyl acetate dropwise, other
Part is consistent.Gained luminosity curve is as shown in Figure 5.
Embodiment 9.
Similar to Example 6, difference is in step 2, by metal halide salt PbBr2Change PbCl into2, other conditions holding
Unanimously.
Embodiment 10.
Similar to Example 6, difference is in step 4, changes ethyl acetate into same volume toluene and hexane mixed solution,
Other conditions are consistent.
Embodiment 11.
Similar to Example 6, difference is in step 4, changes ethyl acetate into toluene, other conditions are consistent.
Embodiment 12.
Similar to Example 6, difference is in step 4, changes ethyl acetate into hexane, other conditions are consistent.
Embodiment 13.
Similar to Example 6, difference is in step 4, changes ethyl acetate into methylene chloride, other conditions keep one
It causes.
Embodiment 14.
Similar to Example 6, difference is in step 4, changes ethyl acetate into isopropanol, other conditions are consistent.
Embodiment 15.
Similar to Example 9, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 16.
Similar to Example 10, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 17.
Similar to Example 11, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 18.
Similar to Example 12, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 19.
Similar to Example 13, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 20.
Similar to Example 14, difference is in step 4, changes 50 μ l of forerunner into 40 μ l, other conditions are consistent.
Embodiment 21.
Similar to Example 15, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 22.
Similar to Example 16, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 23.
Similar to Example 17, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 24.
Similar to Example 18, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 25.
Similar to Example 19, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 26.
Similar to Example 20, difference is in step 4, changes 40 μ l of forerunner into 10 μ l, other conditions are consistent.
Embodiment 27.
Similar to Example 9, difference is in step 2, by metal halide salt PbCl2Change PbI into2, other conditions holding one
It causes.
Embodiment 28.
Similar with embodiment 27, difference is in step 4, by ethyl acetate change into same volume toluene mix with hexane it is molten
Liquid, other conditions are consistent.
Embodiment 29.
Similar with embodiment 27, difference is in step 4, changes ethyl acetate into toluene, other conditions are consistent.
Embodiment 30.
Similar with embodiment 27, difference is in step 4, changes ethyl acetate into hexane, other conditions are consistent.
Embodiment 31.
Similar with embodiment 27, difference is in step 4, changes ethyl acetate into methylene chloride, other conditions keep one
It causes.
Embodiment 32.
Similar with embodiment 27, difference is in step 4, changes ethyl acetate into isopropanol, other conditions are consistent.
Embodiment 33.
Similar to Example 1, difference is the Cs that will be obtained4PbBr6Colloidal solution passes through anion Cl-Displacement obtains
Blue light Cs4PbCl6Colloidal solution, sample solution and luminous spectrum are as shown in Figure 6.
Embodiment 34.
Similar to Example 1, difference is the Cs that will be obtained4PbBr6Colloidal solution passes through anion I-Displacement obtains blue
Light Cs4PbI6Colloidal solution, sample solution and luminous spectrum are as shown in Figure 6.
In short, by adjusting precursor solution infusion volume, adjustable luminous band gap, by Fig. 5, it can be seen that.But not
It will affect its luminescent properties with presoma infusion volume.By anion metathesis, it can get the adjustable preferable luminescent properties of band gap
Colloidal solution.And by changing organic ligand and ratio, the good pure phase perovskite Cs of high volume production, stability is obtained4PbBr6Glue
Liquid solution.
Claims (7)
1. a kind of high quantum production rate zero dimension perovskite structure pure phase Cs4PbBr6Material and synthetic method, which is characterized in that described zero
Tie up pure phase perovskite Cs4PbBr6Reprecipitation method is assisted using ligand, by changing long short hydrocarbon organic ligand, and is changed organic
The ratio of ligand；Include the following steps:
Step 1, by metal halide salt PbBr2It is dissolved in dimethylformamide (DMF) with CsBr, ultrasound makes it completely dissolved；
Step 2, organic ligand is added in the DMF solution for the metal halide salt that step 1 obtains, is reacted after mixing
Precursor solution；
Step 3, reaction precursor liquid solution is rapidly injected or is added dropwise in anti-solvent dropwise, being stirred at room temperature makes fully reacting, most
It is centrifuged afterwards, purification obtains Cs4PbBr6Colloidal solution；
Step 4, by Cs4PbBr6Colloidal solution obtains the Cs of different band gap by anion metathesis4PbCl6With Cs4PbI6Deng
Colloidal solution.
2. preparation method according to claim 1, which is characterized in that step 1, in 4, metal halide salt BX2For lead bromide
(PbBr2), lead iodide (PbI2) or lead chloride (PbCl2), AX is cesium bromide (CsBr).
3. preparation method according to claim 1, which is characterized in that in step 2, the organic ligand is oleic acid and ten
The mixture of diamines, volume ratio are 5:1 ~ 15:1.
4. preparation method according to claim 1, which is characterized in that in step 2, the DMF of the metal halide salt is molten
The volume ratio of liquid and organic ligand mixture is 5:1 ~ 10:1.
5. preparation method according to claim 1, which is characterized in that in step 3, the anti-solvent is ethyl acetate.
6. preparation method according to claim 1, which is characterized in that in step 3, mixing speed 1000r/min, room temperature
Temperature is 25 ~ 30 DEG C.
7. preparation method according to claim 2, which is characterized in that in reaction system, mole of metallic element Pb and Cs
Ratio is 1:1 ~ 1:4.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606505A (en) * | 2019-10-21 | 2019-12-24 | 江苏科技大学 | Zero-dimensional halogen perovskite structure material Cs4PbBr6Preparation and use of |
| CN111944525A (en) * | 2020-08-25 | 2020-11-17 | 深圳大学 | Zero-dimensional cesium-lead-bromine inorganic perovskite material and preparation method thereof |
| CN112877064A (en) * | 2021-01-14 | 2021-06-01 | 中南大学 | Preparation method of pure Cs4PbBr6 perovskite quantum dot and product thereof |
| CN114032098A (en) * | 2021-11-25 | 2022-02-11 | 吉林大学 | Method for improving fluorescence efficiency of zero-dimensional perovskite material |
| CN114507519A (en) * | 2022-04-19 | 2022-05-17 | 南京邮电大学 | Normal-temperature green synthesis method of deep blue perovskite quantum dots and application of deep blue perovskite quantum dots in preparation of perovskite light-emitting diodes |
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2019
- 2019-04-17 CN CN201910306700.6A patent/CN110003900A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110606505A (en) * | 2019-10-21 | 2019-12-24 | 江苏科技大学 | Zero-dimensional halogen perovskite structure material Cs4PbBr6Preparation and use of |
| CN110606505B (en) * | 2019-10-21 | 2022-03-25 | 江苏科技大学 | Zero-dimensional halogen perovskite structure material Cs4PbBr6Preparation and use of |
| CN111944525A (en) * | 2020-08-25 | 2020-11-17 | 深圳大学 | Zero-dimensional cesium-lead-bromine inorganic perovskite material and preparation method thereof |
| CN111944525B (en) * | 2020-08-25 | 2022-05-10 | 深圳大学 | Zero-dimensional cesium-lead-bromine inorganic perovskite material and preparation method thereof |
| CN112877064A (en) * | 2021-01-14 | 2021-06-01 | 中南大学 | Preparation method of pure Cs4PbBr6 perovskite quantum dot and product thereof |
| CN114032098A (en) * | 2021-11-25 | 2022-02-11 | 吉林大学 | Method for improving fluorescence efficiency of zero-dimensional perovskite material |
| CN114032098B (en) * | 2021-11-25 | 2022-11-25 | 吉林大学 | Method for improving fluorescence efficiency of zero-dimensional perovskite material |
| CN114507519A (en) * | 2022-04-19 | 2022-05-17 | 南京邮电大学 | Normal-temperature green synthesis method of deep blue perovskite quantum dots and application of deep blue perovskite quantum dots in preparation of perovskite light-emitting diodes |
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