CN108862376B - A kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution - Google Patents
A kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution Download PDFInfo
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Abstract
The invention discloses a kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution.Select cesium carbonate, lead bromide as reactant, oleic acid, oleyl amine obtain CsPbBr after suitable octadecylene or mineral oil ultrasound is added as surface ligand3Solution.Select cetyl trimethylammonium bromide as cationic surfactant and CsPbBr again3Solution ultrasound 1-2 min, can be obtained the preferable CsPbBr of fluorescent stability3Solution.The still stable CsPbBr of the fluorescence in aqueous solution that this method is prepared3Time used in solution is short, whole that 9 min-14 min(is only needed to include synthesis CsPbBr3The time of perovskite).It is still preferable that the solution prepared directly deposits in fluorescent stability in aqueous solution even phosphate buffer solution, and dispersibility is excellent, and particles in solution is uniform.
Description
Technical field
Present invention relates particularly to a kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution.
Background technique
Full-inorganic perovskite with its higher quantum yield, that emission wavelength can cover entire visible spectrum, halfwidth is opposite
The advantages that relatively narrow, is widely used in the fields such as solar cell module, light emitting diode, sensor.
But current study show that: full-inorganic perovskite is extremely sensitive for polar solvent, especially water-soluble in polar solvent
It disappears in the fluorescence short time in liquid.This characteristic significantly limits the application range of full-inorganic perovskite.It is complete in order to improve
Stability of the inorganic perovskite in polar solvent especially aqueous solution, the raising antihunt means carried out at present have: (1) adopting
With external surface coating method, such as using caged polyhedral oligomeric silsesquioxane embedding perovskite (Chem.Sci.,2016,7:
, but its poor dispersion in aqueous solution 5699)；(2) in-situ surface Protection Code is used, such as makes perovskite using x-ray bombardment
The surface ligand degree of cross linking increase with improve its stability (ACS Nano, 2016,10:1224 1230), but because organic content is excessively high
So that electric conductivity is bad；(3) using the embedding such as new material, such as using mesoporous silicon oxide embedding perovskite (Angew. Chem., 2016,55:7924-7929).But this method has strict requirements for the selection of material itself and has
The synthesis of a little materials takes a long time, not easy to operate.
In conclusion urgent need develops one kind can to improve perovskite nano material in the application field in bio-sensing field
Directly deposit in aqueous solution and be able to maintain the synthesis side of the perovskite nano material of preferable fluorescent stability and good dispersion
Method.This patent is using cetyl trimethylammonium bromide and full-inorganic CsPbBr3The mode of the direct ultrasonic mixing of perovskite solution
Improve its stability in aqueous solution.This method is easy to operate, and directly the solution of acquisition can be placed in water environment, uses
When it is shorter can quickly prepare, reproducible, the solution dispersion of acquisition is good, and agents useful for same cetyl trimethylammonium bromide is cheap
It is easy to get.
Summary of the invention
The purpose of the present invention is to provide a kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution.
Select cesium carbonate, lead bromide as reactant, suitable octadecylene or mineral are being added as surface ligand in oleic acid, oleyl amine
CsPbBr is obtained after oily ultrasound3Solution.Select again cetyl trimethylammonium bromide as cationic surfactant with
CsPbBr3Solution 1 min -2 min of ultrasound, can be obtained the preferable CsPbBr of fluorescent stability3Solution.This method is prepared
The still stable CsPbBr of fluorescence in aqueous solution3Time used in solution is short, whole only to need 9 min -14 min(including closing
At CsPbBr3The time of perovskite).The solution prepared directly deposits in fluorescence in aqueous solution even phosphate buffer solution
Stability is still preferable, and dispersibility is excellent, and particles in solution is uniform.Select cetyl trimethylammonium bromide as sun simultaneously
Ionic surface active agent is relatively cheap.This method is for improving full-inorganic CsPbBr3Perovskite in aqueous solution grind by stability
Studying carefully has great significance.
To achieve the above object, the present invention adopts the following technical scheme:
(1) suitable cesium carbonate, lead bromide powder are weighed, with a certain amount of octadecylene or mineral oil oil sealing, with isolation
Air, then oleic acid, oleyl amine are added into mixed liquor；
(2) mixed solution in (1) is placed in ultrasonic cell disruptor and is ultrasonically treated 8 min -12 min, solution by
It is transparent to gradually become glassy yellow, stop ultrasound up to full-inorganic CsPbBr3Perovskite solution；
(3) a certain amount of cetyl trimethylammonium bromide, 1 min -2 of ultrasound is added in acquired solution in (2)
Min, cetyl trimethylammonium bromide be all dissolved in mixed liquor to get in aqueous solution with high stability completely without
Machine CsPbBr3Perovskite solution；
(4) be added a certain amount of deionized water in (3) in gained mixed liquor, 3 min -5 min of ultrasound, mixed liquor by
Glassy yellow becomes milk green, observes fluorescence intensity change to prove the stability of its fluorescence in aqueous solution.
Distinguishing feature of the invention is:
(1) using cetyl trimethylammonium bromide as cationic surfactant to improve full-inorganic CsPbBr3Calcium titanium
Mine stability in aqueous solution, the full-inorganic CsPbBr after being embedded using cetyl trimethylammonium bromide3Perovskite is directly deposited
It is put in aqueous solution not only that stability is good, fluorescence property is excellent, dispersion performance is excellent, and particles in solution size is uniform.
(2) present invention mixes full-inorganic CsPbBr using the method for ultrasound3Perovskite solution and cetyl trimethyl bromine
Change ammonium, the whole used time is short, only needs 9 min -14 min.
(3) raw material cetyl trimethylammonium bromide is cheap and easy to get and the instrument that uses conveniently is easy to get.
Detailed description of the invention
Fig. 1 is of the present invention in aqueous solution with high stability after cetyl trimethylammonium bromide embeds
Full-inorganic CsPbBr3Perovskite transmission electron microscope picture.
Fig. 2 is of the present invention in aqueous solution with high stability after cetyl trimethylammonium bromide embeds
Full-inorganic CsPbBr3The stability curve figure of perovskite.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments.
Embodiment 1
The lead bromide for weighing 0.05 mmol cesium carbonate, 0.15 mmol rapidly joins 5 mL octadecylenes, 0.25 thereto
ML oleic acid, 0.25 mL oleyl amine obtain clear solution.Above-mentioned solution is placed in ultrasonic cell disruptor and is ultrasonically treated 8 min.
Solution gradually becomes glassy yellow by transparent, stops ultrasound and obtains full-inorganic CsPbBr3Perovskite solution.It is molten to take out above-mentioned glassy yellow
0.0030 g cetyl trimethylammonium bromide, 1 min of ultrasound, until cetyl trimethyl is added in 100 μ L of liquid thereto
Ammonium bromide is all dissolved in mixed liquor.Obtain full-inorganic perovskite solution in aqueous solution with high stability.In order to demonstrate,prove
Its bright fluorescent stability with higher in aqueous solution, CsPbBr of the Xiang Shangshu added with cetyl trimethylammonium bromide3Calcium
The deionized water of 400 μ L, 3 min -5 min of ultrasound are added in titanium ore solution, solution becomes milk green from glassy yellow.This is mixed
Close 1 h of solution fluorescence intensity decline about 3.58%, 2 h decline about 4.31%, 3 h decline about 5.32%.This method be by
CsPbBr3It is directly placed into after mixing with cetyl trimethylammonium bromide to check its fluorescent stability in aqueous solution, it can
To absolutely prove that this method effectively increases the stability of perovskite solution fluorescence in aqueous solution.
In order to further illustrate the present invention the characteristics of, is carried out further using full-inorganic perovskite obtained in embodiment 1
Analysis.
Fig. 1 is to have high stability through cetyl trimethylammonium bromide in aqueous solution described in the embodiment of the present invention 1
Full-inorganic CsPbBr after embedding3The transmission electron microscope picture of perovskite, as can be seen from Figure 1 full-inorganic CsPbBr3Perovskite is by 16
Alkyl trimethyl ammonium bromide is wrapped in inside.Fig. 2 is shown has high stability through cetyl trimethyl in aqueous solution
Full-inorganic CsPbBr after ammonium bromide embedding3The stability curve figure of perovskite, 1 h of mixed solution fluorescence intensity decline are about
3.58%, 2 h decline about 4.31%, 3 h decline about 5.32%.Fig. 2 illustrate be added cetyl trimethylammonium bromide after completely without
Machine CsPbBr3Perovskite can keep preferable fluorescent stability in aqueous solution really.
Embodiment 2
The lead bromide for weighing 0.05 mmol cesium carbonate, 0.15 mmol rapidly joins 5 mL mineral oil, 0.25 thereto
ML oleic acid, 0.25 mL oleyl amine obtain clear solution.Above-mentioned solution is placed in ultrasonic cell disruptor and is ultrasonically treated 10min.
Solution gradually becomes glassy yellow by transparent, stops ultrasound and obtains full-inorganic CsPbBr3Perovskite solution.It is molten to take out above-mentioned glassy yellow
0.0030 g cetyl trimethylammonium bromide, 1 min of ultrasound, until cetyl trimethyl is added in 100 μ L of liquid thereto
Ammonium bromide is all dissolved in mixed liquor.Obtain full-inorganic perovskite solution in aqueous solution with high stability.
Embodiment 3
The lead bromide for weighing 0.05 mmol cesium carbonate, 0.15 mmol rapidly joins 5 mL octadecylenes, 0.25 thereto
ML oleic acid, 0.25 mL oleyl amine obtain clear solution.Above-mentioned solution is placed in ultrasonic cell disruptor and is ultrasonically treated 12
min.Solution gradually becomes glassy yellow by transparent, stops ultrasound and obtains full-inorganic CsPbBr3Perovskite solution.It takes out above-mentioned bright orange
0.0030 g cetyl trimethylammonium bromide, 2 min of ultrasound, until cetyl three are added in 100 μ L of color solution thereto
Methyl bromide ammonium is all dissolved in mixed liquor.Obtain full-inorganic perovskite solution in aqueous solution with high stability.
The foregoing is merely presently preferred embodiments of the present invention, all equivalence changes done according to scope of the present invention patent,
It is all covered by the present invention.
Claims (6)
1. a kind of raising full-inorganic CsPbBr3Perovskite stability approach in aqueous solution, it is characterised in that: the following steps are included:
(1) lead bromide and cesium carbonate are dissolved in octadecylene or mineral oil, add oleic acid, oleyl amine；
(2) step (1) described mixed liquor is ultrasonically treated, obtains full-inorganic CsPbBr3Perovskite solution；
(3) in the CsPbBr of step (2)3Cetyl trimethylammonium bromide is added in perovskite solution, it is sonicated, it will
CsPbBr3Perovskite solution is uniformly mixed to get to fluorescent stabilization in aqueous solution with cetyl trimethylammonium bromide
CsPbBr3Perovskite solution.
2. according to the method described in claim 1, it is characterized by: the molar ratio of lead bromide and cesium carbonate is 3 in step (1):
1。
3. according to the method described in claim 1, it is characterized by: octadecylene or mineral oil and oleic acid, oleyl amine in step (1)
Volume ratio be 20:1:1.
4. according to the method described in claim 1, it is characterized by: sonication treatment time is 8-12 min in step (2).
5. according to the method described in claim 1, it is characterized by: sonication treatment time is 1-2 min in step (3).
6. according to the method described in claim 1, it is characterized by: CsPbBr in step (3)3Perovskite solution and cetyl
The amount ratio of trimethylammonium bromide is 100 μ L:0.0030 g.
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| CN109762554B (en) * | 2019-03-08 | 2021-07-13 | 福州大学 | Method for synthesizing CsPbBr3 perovskite stable in aqueous solution by one-step method |
| CN110079313A (en) * | 2019-04-10 | 2019-08-02 | 济南大学 | A kind of large scale, spherical shape CsPbBr3/SiO2The preparation method of illuminator |
| CN110144217A (en) * | 2019-06-13 | 2019-08-20 | 中国药科大学 | A kind of CsPbBr3/Cs4PbBr6Composite perofskite material and preparation method thereof |
| CN110184056B (en) * | 2019-06-20 | 2021-10-22 | 南京理工大学 | Synthesis method of high-efficiency halogen perovskite quantum dot scintillator for X-ray imaging |
| CN112051249B (en) * | 2020-09-07 | 2021-06-22 | 福州大学 | Sulfanilic acid modified perovskite composite material and application thereof in nitrite detection |
| CN112964687B (en) * | 2021-02-22 | 2022-02-01 | 江南大学 | Fluorescence ratio detection method for determining moisture content in grease based on fluorescent perovskite nano material |
| CN113292096B (en) * | 2021-06-09 | 2022-11-11 | 曲阜师范大学 | Preparation method for synthesizing inorganic perovskite nanocrystal by non-injection one-step method |
| CN115685304B (en) * | 2022-01-18 | 2024-07-02 | 杭州钛光科技有限公司 | Highly stable PQD scintillator and preparation method thereof |
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