CN108793234A - A kind of CsPbX3Quantum dot room temperature synthetic method - Google Patents
A kind of CsPbX3Quantum dot room temperature synthetic method Download PDFInfo
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- CN108793234A CN108793234A CN201810595810.4A CN201810595810A CN108793234A CN 108793234 A CN108793234 A CN 108793234A CN 201810595810 A CN201810595810 A CN 201810595810A CN 108793234 A CN108793234 A CN 108793234A
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Abstract
The invention discloses a kind of CsPbX3Quantum dot room temperature synthetic method, includes the following steps：Cesium carbonate is dissolved in alkane chain organic acid, caesium presoma is made into；Lead bromide and the organic bromination ammonium salt of branched are dissolved in toluene, the stirring and dissolving in air at room temperature obtains lead presoma；DDAB is dissolved in toluene, DDAB solution is obtained；Caesium presoma is injected into lead presoma, is stirred to react, intermediate is obtained；DDAB solution is added into obtained intermediate, is stirred to react, CsPbX is obtained3Quantum dot stoste；The CsPbX that will be obtained3Quantum dot stoste is added purification solvent and is centrifuged, and redisperse obtains CsPbX in organic solvent3Quantum dot.The CsPbX of the present invention3Quantum dot room temperature synthetic method synthesizes the excellent CsPbX of luminescent properties under room temperature using three kinds of ligand coordinated effects to realize3The quantum yield of quantum dot, ink dispersion liquid is more than 90%, while having single pass radiation recombination.
Description
Technical field
The present invention relates to a kind of CsPbX3Quantum dot room temperature synthetic method.
Background technology
CsPbX3Quanta point material because having many advantages, such as high quantum yield, narrow glow peak, higher thermal stability,
The extensive concern of researcher is caused in recent years.In LED component, detector, the photoelectric fields such as solar cell, CsPbX3Amount
Son point has original performance, has boundless foreground.Currently, more classical perovskite quantum dot is all to pass through high temperature
(usually at 120 DEG C or more) hot injection method synthesis, operation is complex and needs inert gas environment.Low temperature or room temperature synthesis
CsPbX3Quantum dot is gradually paid close attention to by people, however the CsPbX of the current room temperature synthesis reported3Although quantum dot fluorescence volume
Sub- yield also reaches requirement, however application effect is very poor in electroluminescent device, is often only used in luminescence generated by light.
Therefore, it is necessary to a kind of CsPbX3Quantum dot room temperature synthetic method is to solve the above problems.
Invention content
The purpose of the present invention is that solve the above-mentioned problems, is provided a kind of without protective gas and in room temperature condition
The high quality CsPbX of lower synthesis3Quantum dot.
The present invention is achieved through the following technical solutions above-mentioned purpose:
A kind of CsPbX3Quantum dot room temperature synthetic method, includes the following steps：
1), cesium carbonate is dissolved in alkane chain organic acid, is made into caesium presoma；By lead bromide and the organic ammonium bromide of branched
Salt is dissolved in toluene, and the stirring and dissolving in air at room temperature obtains lead presoma；DDAB is dissolved in toluene, DDAB is obtained
Solution；
2), caesium presoma is injected into lead presoma, is stirred to react, intermediate is obtained；
3), DDAB solution is added in the intermediate obtained to step 2), is stirred to react, obtain CsPbX3Quantum dot is former
Liquid；
4), the CsPbX for obtaining step 3)3Quantum dot stoste is added purification solvent and is centrifuged, and is redispersed in organic molten
CsPbX is obtained in agent3Quantum dot.
Further, alkane chain organic acid described in step 1) is caprylic acid, n-caproic acid or butyric acid.
Further, a concentration of 0.2-1mol/L of the cesium carbonate in alkane chain organic acid in step 1).
Further, in step 1) the organic bromination ammonium salt of branched be four n-octyl ammonium bromides, four hexyl ammonium bromides or
Four dodecyl bromination ammoniums.
Further, a concentration of 0.02~0.1mol/L of the lead bromide in toluene, branched organic bromine in step 1)
Change a concentration of 0.04~0.2mol/L of the ammonium salt in toluene.
Further, in step 1) DDAB solution a concentration of 0.04~0.06mol/L.
Further, the time being stirred to react in step 2) is 1~5min.
Further, it is ethyl acetate, methyl acetate, butyl acetate, isopropanol, just that solvent is purified described in step 4)
Butanol, the tert-butyl alcohol or acetone.
Further, CsPbX in step 4)3Quantum dot stoste and the volume ratio of purification solvent are 1:(1-3).
Further, organic solvent is n-hexane, normal octane or toluene in step 4).
Advantageous effect：The CsPbX of the present invention3Quantum dot room temperature synthetic method is realized using three kinds of ligand coordinated effects
The excellent CsPbX of synthesis luminescent properties under room temperature3The quantum yield of quantum dot, ink dispersion liquid is more than 90%, simultaneously
With single pass radiation recombination, show the CsPbX of this room temperature procedure synthesis3Quantum dot almost Perfect, luminescent properties and
Crystalline quality is enough the quantum dot to match in excellence or beauty using high warm injection method synthesis.
Description of the drawings
Fig. 1 is the TEM figures of quantum dot prepared by embodiment 1；
Fig. 2 is the XRD x ray diffractions of embodiment 1；
Fig. 3 is embodiment 1, embodiment 2, the PL figures corresponding with the quantum dot that embodiment 4 obtains of embodiment 3；
Fig. 4 is embodiment 1, embodiment 2, the EQE curves corresponding with QLED prepared by embodiment 4 of embodiment 3.
Specific implementation mode
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation describes, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
The invention discloses the inorganic perovskite quantum dots that a kind of room temperature method synthesizes high quality, first prepare caesium presoma, then
By halogenation lead salt and the organic bromination ammonium salt co-dissolve of branched in toluene, mixed caesium presoma is injected into lead presoma
In obtain the weaker perovskite structure of shining, DDAB surface agent precursor solutions are then added and continue stirring and carry out surface to be modified i.e.
The very high perovskite quantum dot of luminous efficiency can be obtained, final CsPbX is obtained finally by centrifugation purification3Quantum dot.It can be with
High performance QLED is constructed using this room temperature synthesis quantum dot.
The device architecture of the present invention is ITO/PEDOT:PSS/PTAA/CsPbX3QDs/TPBi/LiF/Al or ITO/
PEDOT:PSS/Poly-TPD/CsPbX3QDs/TPBi/LiF/Al, wherein PEDOT:PSS, PTAA, Poly-TPD and
CsPbX3QDs layers are constructed by spin-coating method, and TPBi, LiF and Al are constructed by thermal evaporation method.
The invention discloses a kind of CsPbX synthesizing luminescent properties almost Perfect by room temperature3(X is halogen) quantum dot
Preparation method can be used for preparing high-performance quantum dot point luminescent diode (QLED).The present invention is made using three kinds of ligand coordinateds
The excellent CsPbX of luminescent properties is synthesized under room temperature for realizing3The quantum yield of quantum dot, ink dispersion liquid is more than
90%, while there is single pass radiation recombination, show the CsPbX of this room temperature procedure synthesis3Quantum dot almost Perfect, hair
Optical property and crystalline quality are enough the quantum dot to match in excellence or beauty using high warm injection method synthesis.And the quantum dot of this method synthesis is available
In preparing high performance electroluminescent diode apparatus, cleverly short chain ligand collocation does not hinder while ensureing high luminescence energy
Hinder efficient electrical pumping, to obtain the CsPbX of high-luminous-efficiency3Quantum dot light emitting device.
Embodiment 1：
1) 1.2mmol cesium carbonates are dissolved in 3mL octanoic acids, are made into caesium presoma；
2) by 2mmol lead bromides, tetra- n-octyl ammonium bromides of 4.4mmol in 30mL toluene, stirred in air at room temperature to
It is completely dissolved, obtains lead presoma；
3) by 0.6mmol DDAB ultrasonic dissolutions in 10mL toluene；
4) caesium presoma is injected into lead presoma, reacts 3min, the DDAB solution in step 3) is added, continues to stir
2min obtains CsPbBr3Quantum dot stoste；
5) centrifugation of 60mL ethyl acetate is added in quantum dot stoste and gives up supernatant, precipitation is dispersed in 10mL normal octanes
Obtain CsPbBr3Quantum dot.
Using：The spin coating PEDOT successively in the glass substrate for have ITO electrode:PSS, PTAA and CsPbBr3Quantum dot, so
The Al electrodes for evaporating the LiF and 100nm of TPBi, 1nm of 40nm successively in thermal evaporation cavity afterwards, obtain QLED devices.
Embodiment 2：
Using 1 same process of embodiment, difference lies in octanoic acid in the step 1) of embodiment 1 is changed to caproic acid, other conditions
It is consistent.
Embodiment 3：
Using 1 same process of embodiment, difference lies in by four n-octyl ammonium bromides in the step 2) of embodiment 1 be changed to four oneself
Base ammonium bromide, other conditions are consistent.
Embodiment 4：
Using 1 same process of embodiment, difference lies in normal octane in the step 5) of embodiment 1 is changed to n-hexane, other
Condition is consistent.
As it can be seen from fig. 1 that the size of this room-temperature quantum point in 20nm hereinafter, pattern be it is rectangular, as seen from Figure 2,
The synthesized nanocrystalline crystallinity of room temperature is good.The room temperature that Fig. 3 shows synthesis is nanocrystalline with relatively narrow high-purity green luminescence peak
(half-peak breadth is less than 20nm, and luminous peak position is in 514nm or so).From fig. 4, it can be seen that the room-temperature quantum point of this method synthesis,
Even if without further improvement, luminous efficiency highest alreadys exceed 6%, is closed more than known solution at room temperature synthetic method is better than
At CsPbX3Quantum dot.
Claims (10)
1. a kind of CsPbX3Quantum dot room temperature synthetic method, which is characterized in that include the following steps：
1), cesium carbonate is dissolved in alkane chain organic acid, is made into caesium presoma；Lead bromide and the organic bromination ammonium salt of branched is molten
For solution in toluene, the stirring and dissolving in air at room temperature obtains lead presoma；DDAB is dissolved in toluene, DDAB solution is obtained；
2), caesium presoma is injected into lead presoma, is stirred to react, intermediate is obtained；
3), DDAB solution is added in the intermediate obtained to step 2), is stirred to react, obtain CsPbX3Quantum dot stoste；
4), the CsPbX for obtaining step 3)3Quantum dot stoste is added purification solvent and is centrifuged, and redisperse obtains in organic solvent
To CsPbX3Quantum dot.
2. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that alkane chain described in step 1) is organic
Acid is caprylic acid, n-caproic acid or butyric acid.
3. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that cesium carbonate is in alkane chain in step 1)
A concentration of 0.2-1mol/L in organic acid.
4. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that branched organic bromine in step 1)
Change ammonium salt is four n-octyl ammonium bromides, four hexyl ammonium bromides or four dodecyl bromination ammoniums.
5. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that lead bromide is in toluene in step 1)
In a concentration of 0.02~0.1mol/L, a concentration of 0.04~0.2mol/L of the organic bromination ammonium salt of branched in toluene.
6. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that DDAB solution is dense in step 1)
Degree is 0.04~0.06mol/L.
7. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that be stirred to react in step 2) when
Between be 1~5min.
8. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that solvent is purified described in step 4)
For ethyl acetate, methyl acetate, butyl acetate, isopropanol, n-butanol, the tert-butyl alcohol or acetone.
9. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that CsPbX in step 4)3Quantum dot
Stoste and the volume ratio of purification solvent are 1:(1-3).
10. CsPbX as described in claim 13Quantum dot room temperature synthetic method, which is characterized in that organic solvent is just in step 4)
Hexane, normal octane or toluene.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810703A (en) * | 2019-03-04 | 2019-05-28 | 上海应用技术大学 | A kind of CsPbBr3The room temperature preparation method of quantum dot |
| CN110718645A (en) * | 2019-09-24 | 2020-01-21 | 华中科技大学 | Preparation method and product of perovskite quantum dot light-emitting diode |
| CN110846022A (en) * | 2019-11-08 | 2020-02-28 | 南京理工大学 | Polymer composite enhanced CsPbBr3Method for perovskite QLED performance |
| CN111117598A (en) * | 2019-12-19 | 2020-05-08 | 华中科技大学 | ABX based on room temperature methodnY3-nLigand regulation method and application of perovskite nano particles |
| CN111139059A (en) * | 2019-12-19 | 2020-05-12 | 南京理工大学 | Method for improving perovskite quantum dot performance by short-chain alkyl carboxylic acid |
| CN111268724A (en) * | 2020-02-14 | 2020-06-12 | 南京理工大学 | Synthesis of CsPbI by room-temperature nonpolar solvent system3Method for perovskite nanocrystalline |
| CN113075186A (en) * | 2021-03-30 | 2021-07-06 | 泉州师范学院 | Method for detecting zinc dimethyldithiocarbamate based on cesium-lead-bromine quantum dots |
| CN113214830A (en) * | 2021-05-08 | 2021-08-06 | 南京理工大学 | Double-acid assisted synthesis of CsPbX3Method for quantum dots |
| CN116676082A (en) * | 2023-05-29 | 2023-09-01 | 吉林大学 | Method for reconstructing quantum dot surface by polar ligand and realizing high-performance blue light LEDs |
| CN116769479A (en) * | 2023-05-24 | 2023-09-19 | 华南理工大学 | Preparation method of luminescent material based on blue perovskite quantum dots and electroluminescent device thereof |
| CN116925742A (en) * | 2023-07-26 | 2023-10-24 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
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2018
- 2018-06-11 CN CN201810595810.4A patent/CN108793234A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810703A (en) * | 2019-03-04 | 2019-05-28 | 上海应用技术大学 | A kind of CsPbBr3The room temperature preparation method of quantum dot |
| CN110718645A (en) * | 2019-09-24 | 2020-01-21 | 华中科技大学 | Preparation method and product of perovskite quantum dot light-emitting diode |
| CN110846022B (en) * | 2019-11-08 | 2022-09-30 | 南京理工大学 | Polymer composite enhanced CsPbBr 3 Method for perovskite QLED performance |
| CN110846022A (en) * | 2019-11-08 | 2020-02-28 | 南京理工大学 | Polymer composite enhanced CsPbBr3Method for perovskite QLED performance |
| CN111117598A (en) * | 2019-12-19 | 2020-05-08 | 华中科技大学 | ABX based on room temperature methodnY3-nLigand regulation method and application of perovskite nano particles |
| CN111139059A (en) * | 2019-12-19 | 2020-05-12 | 南京理工大学 | Method for improving perovskite quantum dot performance by short-chain alkyl carboxylic acid |
| CN111268724A (en) * | 2020-02-14 | 2020-06-12 | 南京理工大学 | Synthesis of CsPbI by room-temperature nonpolar solvent system3Method for perovskite nanocrystalline |
| CN113075186A (en) * | 2021-03-30 | 2021-07-06 | 泉州师范学院 | Method for detecting zinc dimethyldithiocarbamate based on cesium-lead-bromine quantum dots |
| CN113214830A (en) * | 2021-05-08 | 2021-08-06 | 南京理工大学 | Double-acid assisted synthesis of CsPbX3Method for quantum dots |
| CN116769479A (en) * | 2023-05-24 | 2023-09-19 | 华南理工大学 | Preparation method of luminescent material based on blue perovskite quantum dots and electroluminescent device thereof |
| CN116676082A (en) * | 2023-05-29 | 2023-09-01 | 吉林大学 | Method for reconstructing quantum dot surface by polar ligand and realizing high-performance blue light LEDs |
| CN116925742A (en) * | 2023-07-26 | 2023-10-24 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
| CN116925742B (en) * | 2023-07-26 | 2024-01-30 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
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