CN109370566A - A kind of perovskite quantum dot stability improvement method adjusted based on ligand - Google Patents
A kind of perovskite quantum dot stability improvement method adjusted based on ligand Download PDFInfo
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- CN109370566A CN109370566A CN201811420118.4A CN201811420118A CN109370566A CN 109370566 A CN109370566 A CN 109370566A CN 201811420118 A CN201811420118 A CN 201811420118A CN 109370566 A CN109370566 A CN 109370566A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
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Abstract
The invention discloses a kind of perovskite quantum dot stability improvement methods adjusted based on ligand, comprising the following steps: weighs a certain proportion of lead halide, cesium carbonate is put into reaction vessel；At room temperature, ligand organic acid and ligand organic amine is added；Solvent stability octadecylene is added at room temperature, stirring is mixed；Reaction vessel is subjected to water-bath or certain time is reacted in oil bath, while being vigorously stirred using magnetic stirring apparatus；Product is washed using acetone, removes unreacted presoma and extra ligand, is dried in vacuo by adding isometric n-hexane after centrifugation after concussion dissolution precipitates, obtains inorganic perovskite CsPbX3Quantum dot powder；A kind of perovskite quantum dot stability improvement method adjusted based on ligand of the invention has the advantages that preparation method is simple, preparation cost is low, material is simple, reaction condition easy to reach, and improves inorganic perovskite CsPbX3The anti-polar solvent ability of quantum dot and thermal stability.
Description
Technical field
The present invention relates to quantum dot fields, and in particular to a kind of perovskite quantum dot stability raising adjusted based on ligand
Method.
Background technique
Full-inorganic perovskite is due to its excellent luminescent properties: half-peak width, and quantum yield is high, adjustable band-gap energy,
Therefore it is widely used in solar battery, light emitting diode, laser, photodetector, in the multiple fields such as biosensor.
Although it has so many excellent properties, there is no widely being used in actual production, this is primarily due to existing rank
The perovskite quantum dot of Duan Hecheng is also unstable, including its easily decaying oxidation in air, the easy decaying of fluorescence in polar solvent,
The factors such as thermal stability difference all significantly limit its development.
Present price section has had research to improve its stability, such as reaches waterproof using mesoporous material cladding, uses glue
Body encapsulates perovskite quantum dot, is achieved the effect that keep perovskite stable with composite material etc..But it is all by calcium titanium at all
The principle that mine quantum dot is isolated from the environment still is limited using upper, cannot be solved the problems, such as from this.Therefore from perovskite
Material itself is started with, and by regulating and controlling ligand, the research of the anti-polar solvent of perovskite quantum dot and stability essence is allowed to have ten
Divide great meaning.
Summary of the invention
In view of this, the present invention provides a kind of calcium adjusted based on ligand to solve above-mentioned the problems of the prior art
Titanium ore quantum dot stability improvement method, by adjusting the covered effect of perovskite quantum dot surface ligand, to reach raising
The purpose of full-inorganic perovskite quantum dot anti-polar solvent and thermal stability, does not influence its luminescent properties not only, also inherently
Service performance is improved to enable full-inorganic perovskite quantum dot further to develop.
To achieve the above object, technical scheme is as follows.
A kind of perovskite quantum dot stability improvement method adjusted based on ligand, is included the following steps；
Step 1, weigh a certain proportion of lead halide, cesium carbonate is put into reaction vessel；
Ligand organic acid and ligand organic amine is added in step 2, at room temperature；
Solvent stability octadecylene is added in step 3 at room temperature, stirs 5~10s, is mixed；
Reaction vessel is carried out water-bath or oil bath reaction certain time, while acutely being stirred using magnetic stirring apparatus by step 4
It mixes；
Step 5 washs product using acetone, removes unreacted presoma and excessive ligand, by centrifugation after again
N-hexane is added to be dried in vacuo after concussion dissolution precipitates, obtain inorganic perovskite CsPbX3Quantum dot powder.
Further, the halogen X in the lead halide in the step 1 is Cl, Br or I, the amount of the lead halide is 0.1~
The molar ratio of 1mmol, the lead halide and cesium carbonate is 1~3:1；The reaction vessel is 15ml vial or tri- mouthfuls of 25ml burnings
Bottle.
Further, the room temperature in the step 2 and step 3 is 5~25 DEG C.
Further, the ligand organic acid in the step 2 and ligand organic amine include three kinds into subassembly, specific to wrap
It includes:
A, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is three second of 3- aminopropyl
The volume ratio of oxysilane, the ligand organic acid and ligand organic amine is 1:0.5~2, the ligand organic acid and halogenation
The ratio of lead is 0.5~2ml:0.1mmol；
B, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is the nitridation of class graphite-phase
Carbon (g-C3N4), the class graphite phase carbon nitride is lamellar morphology, and the ratio with lead halide is 0.1g:0.1mmol；
C, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is two containing hydrophilic group
The volume ratio of ethanol amine, the ligand organic acid and ligand organic amine is 1:0.5~2, the ligand organic acid and lead halide
Ratio be 0.5~2ml:0.1mmol.
Further, the ratio of the stabilizer octadecylene in the step 3 and lead halide is 10ml:0.01mmol.
Further, bath temperature is 70~90 DEG C in the step 4, and oil bath temperature is 100~120 DEG C；The magnetic force
The revolving speed of blender is 100~200rmp；When temperature is 70~80 DEG C, the reaction time is 50~60min, when temperature is 90 DEG C
When, the reaction time is 30~40min, and when temperature is 100~120 DEG C, the reaction time is 20~30min.
Further, the ratio of the acetone in the step 5, octadecylene and n-hexane is 1:1:1；Turn when the centrifugation
Speed is 8000~10000rmp, and centrifugation time is 5~10min；The temperature when vacuum drying is 60 DEG C.
Compared with the prior art, the invention has the following beneficial effects:
1, preparation method is simple and convenient, can be with the anti-polar solvent of one-step synthesis and the inorganic perovskite CsPbX having good stability3Amount
Sub-, fluorescence keeps not being quenched for a long time.
2, inorganic perovskite CsPbX is inherently improved3The anti-polar solvent ability of quantum dot and thermal stability.
3, preparation cost is low, and material is simple, and reaction condition is not harsh, can easily send out popularization.
4, the perovskite quantum dot prepared is not needed further to add other composite materials and can be applied.It can greatly mention
It is high its in LED, the application such as display screen is upper.
Detailed description of the invention
Fig. 1 is a kind of process signal of perovskite quantum dot stability improvement method adjusted based on ligand of the invention
Figure.
Fig. 2 is the inorganic perovskite quantum dot Absorption and emission spectra that the embodiment of the present invention 1 synthesizes.
Fig. 3 is the inorganic perovskite quantum dot Absorption and emission spectra that the embodiment of the present invention 2 synthesizes.
Fig. 4 is the decaying schematic diagram of the inorganic perovskite quantum dot of the synthesis of the embodiment of the present invention 1 in ethanol.
Fig. 5 is the inorganic perovskite quantum dot thermal stability schematic diagram that the embodiment of the present invention 2 synthesizes.
Specific embodiment
Specific implementation of the invention is described further below in conjunction with attached drawing and specific embodiment.It may be noted that
It is that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments, based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
As shown in Figure 1, for a kind of stream of perovskite quantum dot stability improvement method adjusted based on ligand of the invention
Journey schematic diagram, comprising the following steps:
Step 1, weigh a certain proportion of lead halide, cesium carbonate is put into reaction vessel；
Ligand organic acid and ligand organic amine is added in step 2, at room temperature；
Solvent stability octadecylene is added in step 3 at room temperature, stirs 5~10s, is mixed；
Reaction vessel is carried out water-bath or oil bath reaction certain time, while acutely being stirred using magnetic stirring apparatus by step 4
It mixes；
Step 5 washs product using acetone, removes unreacted presoma and excessive ligand, by centrifugation after again
N-hexane is added to be dried in vacuo after concussion dissolution precipitates, obtain inorganic perovskite CsPbX3Quantum dot powder.
Embodiment 1
At 25 DEG C, 0.11gPbBr is weighed respectively using balance2And 0.0326gCs2CO3Powder is used in 25ml three-necked flask
5ml needle tubing draws 10ml octadecylene, draws 0.5ml oleic acid and 0.75ml3- aminopropyl triethoxysilane with the small needle tubing of 1ml,
Magnetic stirring apparatus is opened under room temperature, revolving speed 80rpm is evenly stirred until that upper solution is not layered, and color is uniform；
Three-necked flask is placed in 80 DEG C of water-baths, heats while being vigorously stirred, revolving speed gradually increased as 100rpm, reaction time
For 60min, solution is faint yellow in appearance in 15 minutes or so, issues cyan light with the ultraviolet light irradiation of 365nm, and solution has been after 30min
Through turning yellow.System is placed in condition of ice bath after reaction, product is washed using acetone, before removal is unreacted
Body and excessive ligand are driven, is dried in vacuo, is obtained inorganic by adding n-hexane after centrifugation after concussion dissolution precipitates
Perovskite CsPbX3Quantum dot powder.Such as Fig. 2, shown in Absorption and emission spectra curve, Emission Spectrum Peals are located at the left side 480nm
It is right.Fig. 4 is the decaying schematic diagram of the inorganic perovskite quantum dot of the synthesis of the embodiment of the present invention 1 in ethanol.As it can be seen that from essence
On improve inorganic perovskite CsPbX3The anti-polar solvent ability of quantum dot and thermal stability.
Ligand uses oleic acid and 3- aminopropyl triethoxysilane, the straight chain and three ethoxy of 3- aminopropyl that principle passes through oleic acid
The surface ligand that three straight chain of base silane is formed intersects cooperation, so that inorganic perovskite quantum dot surface ligand be made to coat density
Increase, achievees the purpose that crystal inside is protected not destroyed by polar solvent, while enhancing thermal stability.
Embodiment 2
At 25 DEG C, 0.11gPbBr is weighed respectively using balance2And 0.0326gCs2CO3Powder is used in 25ml three-necked flask
5ml needle tubing draws 10ml octadecylene, draws 0.25ml acetic acid with the small needle tubing of 1ml, and weigh 0.05g class graphite phase carbon nitride
(g-C3N4), magnetic stirring apparatus is opened under room temperature, and revolving speed 80rpm is evenly stirred until that upper solution is not layered, and color is uniform；
Three-necked flask is placed in 90 DEG C of water-baths, heats while being vigorously stirred, revolving speed was gradually increased to as 200rpm, reaction time
For 40min, solution is faint yellow in appearance in 10 minutes or so, issues cyan light with the ultraviolet light irradiation of 365nm, and solution has been after 20min
Through turning yellow.After reaction, product is washed using acetone in system ice bath 5 seconds, remove unreacted presoma and
Excessive ligand is dried in vacuo by adding n-hexane after centrifugation after concussion dissolution precipitates, obtains inorganic perovskite
CsPbX3Quantum dot powder.Such as Fig. 3, shown in Absorption and emission spectra curve, Emission Spectrum Peals are located at 520nm or so.
Ligand uses acetic acid and class graphite phase carbon nitride (g-C3N4), acetic acid accelerates carbonic acid by reacting rapidly with cesium carbonate
Caesium dissolution, while being cooperated by the compound with NH2- group of the acetic acid of short chain and sheet, reach preferably fixed and stablized
Inorganic perovskite quantum dot enhances the ability and thermal stability of its anti-polar solvent.Such as Fig. 5, heat stability testing statistics indicate that,
The product is got well than the product thermostabilization normally synthesized.
Embodiment 3
At 25 DEG C, 0.11gPbBr is weighed respectively using balance2And 0.0326gCs2CO3Powder is used in 25ml three-necked flask
5ml needle tubing draws 10ml octadecylene, draws 0.5ml octanoic acid and 0.5ml diethanol amine with the small needle tubing of 1ml, opens magnetic under room temperature
Power blender, revolving speed 80rpm are evenly stirred until that upper solution is not layered, and color is uniform；
Three-necked flask is placed in 90 DEG C of water-baths, heating while being vigorously stirred, revolving speed is gradually upgraded to 200rpm, and the reaction time is
40min, solution is faint yellow in appearance in 10 minutes or so, issues cyan light with the ultraviolet light irradiation of 365nm, and solution has been after 20min
It turns yellow.System ice bath 5 seconds after reaction wash product using acetone, remove unreacted presoma and mistake
The ligand of amount is dried in vacuo by adding n-hexane after centrifugation after concussion dissolution precipitates, obtains inorganic perovskite
CsPbX3Quantum dot powder.
For ligand using octanoic acid and diethanol amine, principle is mainly to pass through the hydrophilic and hydrophobic for changing surface ligand, passes through enhancing
The hydrophily of inorganic perovskite quantum dot surface ligand, to enhance its stability in polar solvent, effect is referring to real
Apply example 2.
In conclusion a kind of perovskite quantum dot stability improvement method adjusted based on ligand of the invention has preparation
Method is simple, preparation cost is low, material is simple, reaction condition easy to reach advantage, and improves inorganic perovskite quantum dot
Anti- polar solvent ability and thermal stability.
Claims (10)
1. a kind of perovskite quantum dot stability improvement method adjusted based on ligand, which comprises the following steps:
Lead halide, cesium carbonate are put into reaction vessel by step 1；
Ligand organic acid and ligand organic amine is added in step 2, at room temperature；
Solvent stability octadecylene is added in step 3 at room temperature, is stirred mixing；
Reaction vessel is carried out water-bath or oil bath reaction, while being stirred using magnetic stirring apparatus by step 4；
Step 5 washs product using acetone, removes unreacted presoma and extra oleic acid oleyl amine, after centrifugation again
N-hexane is added to be dried in vacuo after concussion dissolution precipitates, obtain inorganic perovskite CsPbX3Quantum dot powder.
2. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
Be: halogen X in the lead halide in the step 1 is Cl, Br or I, and the molar ratio of the lead halide and cesium carbonate is 1~3:
1。
3. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
Be: the amount of the lead halide is 0.1~1mmol.
4. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
Be: the room temperature in the step 2 and step 3 is 5~25 DEG C；The time of stirring described in step 2 is 5~10s.
5. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, the ligand organic acid and ligand organic amine in the step 2 include three kinds into subassembly, it specifically includes:
A, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is three second of 3- aminopropyl
The volume ratio of oxysilane, the ligand organic acid and ligand organic amine is 1:0.5~2, the ligand organic acid and halogenation
The ratio of lead is 0.5~2ml:0.1mmol；
B, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is the nitridation of class graphite-phase
Carbon (g-C3N4), the class graphite phase carbon nitride is lamellar morphology, and the ratio with lead halide is 0.1g:0.1mmol；
C, the ligand organic acid is straight-chain acid, including acetic acid, octanoic acid or oleic acid, and the ligand organic amine is two containing hydrophilic group
The volume ratio of ethanol amine, the ligand organic acid and ligand organic amine is 1:0.5~2, the ligand organic acid and lead halide
Ratio be 0.5~2ml:0.1mmol.
6. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, the ratio of stabilizer octadecylene and lead halide in the step 3 is 10ml:0.01mmol.
7. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, bath temperature is 70~90 DEG C in the step 4, and oil bath temperature is 100~120 DEG C；When temperature is 70~80 DEG C, instead
It is 50~60min between seasonable, when temperature is 80~90 DEG C, the reaction time is 30~40min, when temperature is 100~120 DEG C
When, the reaction time is 20~30min.
8. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, the revolving speed of magnetic stirring apparatus described in step 4 is 100~200rmp.
9. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, the volume ratio of acetone, octadecylene and n-hexane in the step 5 is 1:1:1；The revolving speed when centrifugation is 8000
~10000rmp, centrifugation time are 5~10min.
10. a kind of perovskite quantum dot stability improvement method adjusted based on ligand according to claim 1, feature
It is, reaction vessel described in step 4 is 15ml vial or 25ml three-necked flask, and temperature when being dried in vacuo described in step 5 is
60℃。
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| CN110394194A (en) * | 2019-08-07 | 2019-11-01 | 浙江师范大学 | A kind of novel photocatalyst controllable method for preparing based on mineral ligand modification |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| WO2020235420A1 (en) * | 2019-05-21 | 2020-11-26 | Dic株式会社 | Method for producing light emitting particles, light emitting particles, light emitting particle dispersion, ink composition and light emitting element |
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| WO2020235420A1 (en) * | 2019-05-21 | 2020-11-26 | Dic株式会社 | Method for producing light emitting particles, light emitting particles, light emitting particle dispersion, ink composition and light emitting element |
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| CN110255607A (en) * | 2019-07-10 | 2019-09-20 | 景德镇陶瓷大学 | A kind of high stability cross CsPbBr3The nanocrystalline preparation method of perovskite and its product obtained |
| CN110394194A (en) * | 2019-08-07 | 2019-11-01 | 浙江师范大学 | A kind of novel photocatalyst controllable method for preparing based on mineral ligand modification |
| CN111518558A (en) * | 2019-12-11 | 2020-08-11 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN111518558B (en) * | 2019-12-11 | 2021-10-26 | 南京大学 | C3N4Nanosphere loaded all-inorganic perovskite CsPbBr3Preparation method of (1) and electrochemiluminescence cell sensing thereof |
| CN114557478A (en) * | 2022-01-12 | 2022-05-31 | 华南师范大学 | Photocatalytic degradation filter cigarette holder and preparation method thereof |
| CN116333734A (en) * | 2023-03-28 | 2023-06-27 | 电子科技大学 | Perovskite nanocrystalline-based material and preparation method thereof |
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Application publication date: 20190222 |