CN107697946A - A kind of preparation method of full-inorganic perovskite quantum dot - Google Patents
A kind of preparation method of full-inorganic perovskite quantum dot Download PDFInfo
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- CN107697946A CN107697946A CN201711069971.1A CN201711069971A CN107697946A CN 107697946 A CN107697946 A CN 107697946A CN 201711069971 A CN201711069971 A CN 201711069971A CN 107697946 A CN107697946 A CN 107697946A
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Abstract
The present invention provides a kind of preparation method of full-inorganic perovskite quantum dot, is related to technical field of material.Wherein, this method includes：110~145mg metal halide and 2.5~32mg Cs compounds are mixed, and add 5~150mL octadecylene, 0.2~2mL amine organic matter and 0.2~2mL oleic acid wiring solution-forming, and in 80~110 DEG C of 0.2~2h of conditioned response, add 10~15mL precipitating reagent, centrifugation, supernatant is removed, and adds 10~15mL dispersant, is dried to obtain the solution of full-inorganic perovskite quantum dot.Reaction temperature needed for this method is low, it is not necessary to which using inert gas shielding, preparation process is simple, is adapted to large-scale production.
Description
Technical field
The invention belongs to technical field of material, more particularly to a kind of preparation method of perovskite quantum dot.
Background technology
Ca-Ti ore type quantum dot is because its quantum efficiency is high, transmitting peak width is small and glow color is in visible-range
The features such as continuously adjustabe, Ca-Ti ore type quantum dot are considered as in fields such as LED, display, solar cells with potential huge
Using particularly in LED field, being expected to substitute currently used OLED and QLED, turn into the main skill of flexible LED of future generation
Art.
At present, perovskite quantum dot (CsPbX3) preparation method use hot injection method, this method is mainly in 160-200
The precursor solution containing Cs is injected into the precursor solution containing Pb rapid reaction between DEG C temperature and obtains CsPbX3Quantum dot.
But the reaction temperature of this method height under inert atmosphere protection, it is necessary to carry out, therefore be not suitable for large-scale
Technique productions.
The content of the invention
The present invention provides a kind of preparation method of full-inorganic perovskite quantum dot, it is intended to solves existing full-inorganic perovskite
Quantum dot need inert atmosphere protection and, preparation process is complicated, the problem of being not suitable for large-scale technique productions.
The present invention provides a kind of preparation method of full-inorganic perovskite quantum dot, and methods described includes：
By metal halide and Cs compounds according to mol ratio 3:1 mixing, add octadecylene, amine organic matter and oleic acid and be made into
Solution, and in 80~110 DEG C of 0.2~2h of conditioned response, wherein, metal halide is Pb halide or Sn halide, 18
The dosage of alkene, amine organic matter and oleic acid be respectively 50~1500mL/g of metal halide and Cs compound gross masses, 0.2~
2mL/g and 0.2~2mL/g；
Add precipitating reagent, centrifuge, remove supernatant, and add dispersant, be dried to obtain the molten of full-inorganic perovskite quantum dot
Liquid, wherein, the dosage of precipitating reagent and dispersant is metal halide and 10~15mL/g of Cs compound gross masses.
A kind of preparation method of full-inorganic perovskite quantum dot provided by the invention, the reaction temperature needed for this method is low,
Inert gas shielding and cleaning need not be utilized, preparation process is simple, is adapted to large-scale production.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention.
Fig. 1 is the X-ray diffraction test chart for the perovskite quantum dot that the embodiment of the present invention 1 is prepared；
Fig. 2 is the transmissioning electric mirror test figure for the perovskite quantum dot that the embodiment of the present invention 1 is prepared；
Fig. 3 is the transmission electron microscope picture for the perovskite quantum dot that the embodiment of the present invention 2 is prepared；
Fig. 4 is the fluoroscopic examination figure for the perovskite quantum dot that the embodiment of the present invention 2 is prepared；
Fig. 5 is the fluoroscopic examination figure for the perovskite quantum dot that the embodiment of the present invention 3 is prepared；
Fig. 6 is the transmission electron microscope picture for the perovskite quantum dot that the embodiment of the present invention 4 is prepared；
Fig. 7 is the fluorescence spectrum test chart for the perovskite quantum dot that the embodiment of the present invention 4 is prepared；
Fig. 8 is the transmissioning electric mirror test figure for the perovskite quantum dot that the embodiment of the present invention 5 is prepared.
Embodiment
To enable goal of the invention, feature, the advantage of the present invention more obvious and understandable, below in conjunction with the present invention
Accompanying drawing in embodiment, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described reality
It is only part of the embodiment of the present invention to apply example, and not all embodiments.Based on the embodiment in the present invention, people in the art
The every other embodiment that member is obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
The present invention provides a kind of preparation method of full-inorganic perovskite quantum dot, and this method includes：
Step 1: by metal halide and Cs compounds according to mol ratio 3:1 mixing, add octadecylene, amine organic matter and
Oleic acid wiring solution-forming, and in 80~110 DEG C of 0.2~2h of conditioned response.
Wherein, metal halide is Pb halide or Sn halide, and the dosage of octadecylene, amine organic matter and oleic acid is respectively
50~1500mL/g, 0.2~2mL/g and the 0.2~2mL/g of metal halide and Cs compound gross masses
Step 2: plus precipitating reagent, centrifugation, remove supernatant, and add dispersant, be dried to obtain full-inorganic perovskite quantum
The solution of point.
Wherein, the dosage of precipitating reagent and dispersant is metal halide and 10~15mL/g of Cs compound gross masses.
Specifically, in step 1, Pb halide is PbCl2、PbBr2And PbI2At least one of.Cs compounds are carbonic acid
At least one of caesium, cesium hydroxide, cesium acetate.Amine organic matter is oleyl amine, lauryl amine or n-octyl amine.Preferably, amine organic matter
For oleyl amine.
Preferably, the temperature in step 1 is 90 DEG C, reaction time 0.5h.
Specifically, the solvent in step 2 is acetone, ethanol or chloroform.Preferably acetone.Precipitating reagent be acetone, acetonitrile or
Ethyl acetate.Dispersant is toluene, chloroform, n-hexane or hexamethylene.During centrifugation, the centrifuge parameters that use for 7000~
10000 revs/min, centrifugation time is 5~10min.Preferably, centrifuge parameters are 3000 revs/min, and centrifugation time is
5min。
A kind of preparation method of full-inorganic perovskite quantum dot provided by the invention, the reaction temperature needed for this method is low,
Inert gas shielding need not be utilized, preparation process is simple, is adapted to large-scale production.
Embodiment 1
1) 110mgPbBr is weighed2And 32.5mgCs2CO3Powder is put into round-bottomed flask, then add 10mL octadecylenes,
0.5mL oleyl amines and 0.5mL oleic acid.The solution prepared is heated to 90 DEG C, it is after reaction terminates, solution is cold 0.5 hour during reaction
But to pouring out after room temperature.
2) 10mL acetone is added in solution, 5min is centrifuged on 8000 revs/min of centrifuge, remove supernatant, and add
Enter 10mL n-hexanes, the perovskite quantum dot to precipitate is disperseed again.
3) again scattered solution is centrifuged 5 minutes on 3000 revs/min of centrifuge, pours out green supernatant, i.e.,
To have disperseed the solution of full-inorganic perovskite quantum dot, by the solution of full-inorganic perovskite quantum dot in 60 DEG C of vacuum drying oven
Drying, obtained full-inorganic perovskite quantum dot powder.
X-ray diffraction test and transmissioning electric mirror test are carried out to obtained full-inorganic perovskite quantum dot, such as Fig. 1 and Fig. 2
It is shown.As seen from Figure 1, the full-inorganic perovskite quantum dot that embodiment 1 is prepared has perovskite structure, and free from admixture
Produce.Its average grain diameter is 13nm it can be seen from pattern test figure in Fig. 2.
Embodiment 2
1) 41.7mg PbCl are weighed2、55mg PbBr2With 2.5mg Cs2CO3Powder is put into round-bottomed flask, is then added
10mL octadecylenes, 0.5mL tri octyl phosphines, 1mL oleyl amines and 1mL oleic acid.The solution prepared is heated to 95 DEG C, 0.5 is small during reaction
When, after reaction terminates, poured out after solution is cooled into room temperature.
2) 10mL ethyl acetate is added in solution, 5min is centrifuged on 8000 revs/min of centrifuge, remove supernatant,
And 10mL hexamethylenes are added, the perovskite quantum dot to precipitate is disperseed again.
3) again scattered solution is centrifuged 5 minutes on 3000 revs/min of centrifuge, pours out green supernatant, i.e.,
To have disperseed the solution of full-inorganic perovskite quantum dot, by the solution of full-inorganic perovskite quantum dot in 60 DEG C of vacuum drying oven
Drying, obtained full-inorganic perovskite quantum dot powder.
Transmission electron microscope and fluorescence spectrum test are carried out to obtained perovskite quantum dot, as shown in Figure 3 and Figure 4.Wherein, by
It is Tetragonal that Fig. 3, which can be seen that perovskite quantum dot, average grain diameter 11nm, fluorescence light is done in the case where 400 nanometers of uviol lamps excite
Spectrum test, emission peak 461nm, peak width is only 12nm, shows superior optical property.
Embodiment 3
1) 55mgPbBr is weighed2、69.1mg PbI2With 20.3mg CsCH3COO powder is put into round-bottomed flask, Ran Houjia
Enter 10mL octadecylenes, 0.5mL oleyl amines and 0.5mL oleic acid.The solution prepared is heated to 100 DEG C, 0.5 hour during reaction, reaction
After end, poured out after solution is cooled into room temperature.
2) 15mL acetone is added in solution, 5min is centrifuged on 7000 revs/min of centrifuge, remove supernatant, and add
Enter 15mL toluene, the perovskite quantum dot to precipitate is disperseed again.
3) again scattered solution is centrifuged 5 minutes on 5000 revs/min of centrifuge, pours out red supernatant, i.e.,
To have disperseed the solution of full-inorganic perovskite quantum dot, by the solution of full-inorganic perovskite quantum dot in 60 DEG C of vacuum drying oven
Drying, obtained full-inorganic perovskite quantum dot powder.
Fluorescence spectrum test is carried out to obtained perovskite quantum dot, as shown in Figure 5.Fig. 5 is to swash in 400 nanometers of uviol lamps
The fluorescence spectrum test given, emission peak 614nm, peak width 40nm, shows superior optical property.
Embodiment 4
1) 83.5mgSnBr is weighed2It is put into 30mg CsOH powder in beaker, then adds 10mL octadecylenes, 0.5mL oil
Amine and 0.5mL oleic acid.The solution prepared is heated to 90 DEG C, 0.5 hour during reaction, after reaction terminates, solution is cooled to room
Poured out after temperature.
2) 12mL acetone is added in solution, 5min is centrifuged on 7000 revs/min of centrifuge, remove supernatant, and add
Enter 13mL n-hexanes, the perovskite quantum dot to precipitate is disperseed again.
3) again scattered solution is centrifuged 5 minutes on 5000 revs/min of centrifuge, pours out supernatant, as divide
The solution of full-inorganic perovskite quantum dot has been dissipated, the solution of full-inorganic perovskite quantum dot has been dried in 60 DEG C of vacuum drying oven
It is dry, obtained full-inorganic perovskite quantum dot powder.
Transmissioning electric mirror test and fluorescence spectrum test are carried out to obtained perovskite quantum dot, as shown in Figure 6 and Figure 7.
Embodiment 5
1) 110mgPbBr is weighed2It is put into round-bottomed flask, then adds 5mL octadecylenes, 0.5mL oleyl amines and 0.5mL oil
Acid.The solution prepared is heated to 90 DEG C, makes PbBr2Powder is completely dissolved.
2) 30mg CsOH are weighed to be put into round-bottomed flask, then adds 5 milliliters of octadecylenes and 0.25 milliliter of oleic acid.It will match somebody with somebody
Good solution is heated to 90 DEG C, is completely dissolved CsOH powder.
3) by step 1) and 2) in solution mix, during reaction after 0.5 hour, poured out after solution is cooled into room temperature.
4) 13mL acetone is added in solution, 5min is centrifuged on 7000 revs/min of centrifuge, remove supernatant, and add
Enter 11mL n-hexanes, the perovskite quantum dot to precipitate is disperseed again.
5) again scattered solution is centrifuged 5 minutes on 3000 revs/min of centrifuge, pours out supernatant, as divide
The solution of full-inorganic perovskite quantum dot has been dissipated, the solution of full-inorganic perovskite quantum dot has been dried in 60 DEG C of vacuum drying oven
It is dry, obtained full-inorganic perovskite quantum dot powder.
Transmissioning electric mirror test is carried out to obtained perovskite quantum dot, as shown in Figure 8.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (7)
1. a kind of preparation method of full-inorganic perovskite quantum dot, it is characterised in that methods described includes：
By metal halide and Cs compounds according to mol ratio 3:1 mixing, addition octadecylene, amine organic matter and oleic acid are made into molten
Liquid, and in 80~110 DEG C of 0.2~2h of conditioned response, wherein, metal halide is Pb halide or Sn halide, octadecylene,
The dosage of amine organic matter and oleic acid is respectively metal halide and 50~1500mL/g, the 0.2~2mL/g of Cs compound gross masses
And 0.2~2mL/g；
Add precipitating reagent, centrifuge, remove supernatant, and add dispersant, be dried to obtain the solution of full-inorganic perovskite quantum dot, its
In, the dosage of precipitating reagent and dispersant is metal halide and 10~15mL/g of Cs compound gross masses.
2. according to the method for claim 1, it is characterised in that the Pb halide is PbCl2、PbBr2And PbI2In extremely
Few one kind.
3. according to the method for claim 1, it is characterised in that the Sn halide is SnCl2、SnBr2And SnI2In extremely
Few one kind.
4. according to the method for claim 1, it is characterised in that the Cs compounds are cesium carbonate, cesium hydroxide, cesium acetate
At least one of.
5. according to the method for claim 1, it is characterised in that the dispersant is toluene, chloroform, n-hexane or hexamethylene
Alkane.
6. according to the method for claim 1, it is characterised in that the precipitating reagent is acetone, acetonitrile or ethyl acetate.
7. according to the method for claim 1, it is characterised in that the amine organic matter is oleyl amine, lauryl amine or n-octyl amine.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217718A (en) * | 2018-03-13 | 2018-06-29 | 南方科技大学 | A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes |
| CN108504356A (en) * | 2018-05-14 | 2018-09-07 | 华中科技大学 | One kind mixing inorganic halogen perovskite quantum dot of manganese and the preparation method and application thereof |
| CN108862376A (en) * | 2018-09-17 | 2018-11-23 | 福州大学 | A kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution |
| CN109950398A (en) * | 2019-01-22 | 2019-06-28 | 湖南大学 | A kind of photodetector of ultraviolet light and preparation method thereof |
| CN110922968A (en) * | 2019-12-23 | 2020-03-27 | 宁波大学 | Preparation method of all-inorganic perovskite quantum dot used as blue-violet light source |
| CN111170649A (en) * | 2018-11-09 | 2020-05-19 | 上海交通大学 | Method for preparing cesium-based all-inorganic perovskite material through low-temperature reaction |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108217718A (en) * | 2018-03-13 | 2018-06-29 | 南方科技大学 | A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes |
| CN108504356A (en) * | 2018-05-14 | 2018-09-07 | 华中科技大学 | One kind mixing inorganic halogen perovskite quantum dot of manganese and the preparation method and application thereof |
| CN108504356B (en) * | 2018-05-14 | 2020-08-18 | 华中科技大学 | Manganese-doped inorganic halogen perovskite quantum dot and preparation method and application thereof |
| CN108862376A (en) * | 2018-09-17 | 2018-11-23 | 福州大学 | A kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution |
| CN111170649A (en) * | 2018-11-09 | 2020-05-19 | 上海交通大学 | Method for preparing cesium-based all-inorganic perovskite material through low-temperature reaction |
| CN109950398A (en) * | 2019-01-22 | 2019-06-28 | 湖南大学 | A kind of photodetector of ultraviolet light and preparation method thereof |
| CN110922968A (en) * | 2019-12-23 | 2020-03-27 | 宁波大学 | Preparation method of all-inorganic perovskite quantum dot used as blue-violet light source |
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