CN109796775B - Perovskite quantum dot functionalized fluorescent paraffin and preparation method thereof - Google Patents
Perovskite quantum dot functionalized fluorescent paraffin and preparation method thereof Download PDFInfo
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- CN109796775B CN109796775B CN201910069579.XA CN201910069579A CN109796775B CN 109796775 B CN109796775 B CN 109796775B CN 201910069579 A CN201910069579 A CN 201910069579A CN 109796775 B CN109796775 B CN 109796775B
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Abstract
The invention discloses perovskite quantum dot functionalized fluorescent paraffin and a preparation method thereof. The perovskite quantum dot functionalized fluorescent paraffin has high fluorescent quantum efficiency, has good stability to air and water vapor, has wide application prospect, and can be applied to preparation of fluorescent paraffin toys, fluorescent candles, fluorescent crayons, fluorescent waxed paper and the like.
Description
Technical Field
The invention belongs to the technical field of nano and functional materials, and particularly relates to perovskite quantum dot functionalized fluorescent paraffin and a preparation method thereof.
Background
Perovskite quantum dots, including all-inorganic or organic and inorganic hybrid perovskite quantum dots, are novel materials which have been developed in recent years, have extremely high quantum efficiency and good photoelectric property, are greatly concerned in the world, and have wide application prospects in the fields of solar cells, Light Emitting Diodes (LEDs), photoelectric detectors, lasers, chemical and biological sensing, fluorescent materials and the like. However, perovskite quantum dots also have some obvious disadvantages, for example, perovskite quantum dots which are extremely unstable to oxygen, water vapor and aqueous solution in air and are easy to degrade and decompose have great limitation on application of perovskite quantum dots with excellent photoelectric properties.
The invention adopts the paraffin, which is a material frequently used in industry and daily life, to protect the perovskite quantum dots with water and gas sensitivity, prepares the perovskite quantum dot functionalized fluorescent paraffin, and utilizes the good hydrophobicity, gas tightness and chemical stability of the paraffin to realize the effective protection of the perovskite quantum dots, thereby greatly improving the stability of the perovskite quantum dots and simultaneously keeping the original excellent optical properties. The perovskite quantum dots synthesized by the organic phase have good lipophilicity, can be uniformly dispersed in various paraffin materials, have the advantages of wide excitation and narrow emission, are multiple in color, high in purity and high in fluorescence intensity, can be used for preparing perovskite quantum dot functionalized fluorescent paraffin with various colors and good performance, have wide application prospect, and can be applied to preparing fluorescent paraffin toys, fluorescent candles, fluorescent crayons, fluorescent waxed paper, fluorescent powder and the like.
Disclosure of Invention
The invention aims to provide perovskite quantum dot functionalized fluorescent paraffin and a preparation method thereof, which are simple to operate and relatively low in cost, and the prepared perovskite quantum dot functionalized fluorescent paraffin has the advantages of high fluorescent quantum yield, good stability, multiple colors, wide application and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the perovskite quantum dot functionalized fluorescent paraffin comprises the following steps:
(1) dispersing the perovskite quantum dots by using an organic solution to prepare a uniformly dispersed perovskite quantum dot organic solution;
(2) controlling the temperature of the paraffin above the melting point by heating and stirring to melt the paraffin into liquid;
(3) injecting the perovskite quantum dot organic solution obtained in the step (1) into the liquid paraffin obtained in the step (2), and fully stirring and mixing the solution under the condition of keeping the paraffin molten state to obtain a uniform perovskite quantum dot-organic solvent-paraffin mixed solution;
(4) putting the mixed solution obtained in the step (3) into a vacuum drying oven, and removing the organic solvent under reduced pressure under the condition of maintaining a molten state to obtain a perovskite quantum dot-paraffin solution;
(5) and (4) cooling the perovskite quantum dot-paraffin solution obtained in the step (4) to room temperature to obtain the perovskite quantum dot functionalized fluorescent paraffin.
The perovskite quantum dots are all inorganic or organic and inorganic hybrid perovskite quantum dots, and the fluorescence of the perovskite quantum dots is green, blue, red or a mixed color of more than two colors.
The organic solvent comprises volatile organic solvents such as n-hexane and the like.
The paraffin is one or more of low-melting-point paraffin, high-melting-point paraffin, liquid paraffin or paraffin derivatives.
The obtained perovskite functionalized fluorescent paraffin is applied to the preparation of products such as fluorescent paraffin toys, fluorescent candles, fluorescent crayons, fluorescent waxed paper, fluorescent powder and the like.
The invention has the following remarkable advantages:
(1) according to the invention, perovskite quantum dots with high fluorescence quantum yield are adopted for functional modification, and paraffin with strong fluorescence performance is obtained. The hydrophobic groups on the surface of the perovskite quantum dots can enable the fluorescent substance to be uniformly dispersed in paraffin, and the paraffin has excellent hydrophobicity and air tightness and can effectively protect the perovskite quantum dots so as to keep the long-term fluorescence stability.
(2) The invention has the characteristics of relatively cheap and easily obtained raw materials, simple and convenient production process, high yield and the like. The prepared perovskite quantum dot functionalized paraffin has strong fluorescence intensity, stable performance, no change of the original properties of the paraffin and wide application prospect.
Drawings
Fig. 1 is a picture of fluorescent perovskite quantum dot organic solutions with different colors under the irradiation of white light (left) and ultraviolet light (right) (blue fluorescent perovskite quantum dots, green fluorescent perovskite quantum dots and red fluorescent perovskite quantum dots are sequentially arranged according to the sequence of up, middle and down).
Fig. 2 is a low-resolution transmission electron micrograph (a) and a high-resolution transmission electron micrograph (B) of the perovskite quantum dot nanocrystal.
Fig. 3 is a picture of prepared different color perovskite quantum dot functionalized fluorescent paraffin under white light (a) and ultraviolet light (B), wherein, (a) blue fluorescent perovskite quantum dot functionalized fluorescent paraffin; (b) green fluorescent perovskite quantum dot functionalized fluorescent paraffin; (c) the red fluorescent perovskite quantum dot functionalized fluorescent paraffin.
Fig. 4 is a sample diagram of a colored fluorescent paraffin cartoon toy made of different colored perovskite quantum dot functionalized fluorescent paraffins, wherein (a) is blue, (B) is green, and (C) is red.
Fig. 5 is a sample diagram of color phosphor powder made of different color perovskite quantum dot functionalized fluorescent paraffin, wherein, (a 1), (B1) and (C1) are respectively pictures of blue, green and red paraffin phosphor powder under white light, and (a 2), (B2) and (C2) are respectively pictures of blue, green and red paraffin phosphor powder under ultraviolet light.
Fig. 6 is a sample diagram of a color LED bulb made of paraffin fluorescent powder functionalized by perovskite quantum dots of different colors, wherein (a), (b), (c) and (d) are respectively pictures before the blue, green, red and white LEDs are powered on, and (e), (f), (g) and (h) are respectively pictures when the blue, green, red and white LEDs are powered on.
Detailed Description
In order to make the present invention more comprehensible, the technical solutions of the present invention are further described below with reference to specific embodiments, but the present invention is not limited thereto.
Example 1
The synthesis method of the green fluorescent perovskite quantum dot comprises the following steps: under the protection of nitrogen, 5 mL of octadecene and 0.188 mmol of PbBr are added into a reaction flask20.5 mL oleic acid and 0.5 mLOleylamine, heated to 120 ℃ for 1 hour to remove water; then the temperature is raised to 160 ℃ when PbBr is present2And after complete dissolution, 0.4 mL of cesium oleate which is heated to 120 ℃ in advance is injected into the reaction flask, after a few seconds, the reaction flask is rapidly cooled by using an ice bath, the reaction solution is centrifuged at 10000 r/min, clear liquid is removed, the obtained precipitate is green fluorescent perovskite quantum dots, and 5 mL of n-hexane is used for dispersing the green fluorescent perovskite quantum dots for later use.
The synthesis method of the blue and red fluorescent perovskite quantum dots is similar to that of the green fluorescent perovskite quantum dots, except that PbBr is respectively used2-PbCl2Mixture (0.094 mmol PbBr)2+0.094 mmol PbCl2) And PbBr2-PbI2Mixture (0.075 mmol PbBr)2+0.113 mmol PbI2) Replace simply used PbBr2（0.188 mmol）。
The picture of the synthesized three-color fluorescent perovskite quantum dot organic solution under the irradiation of white light and ultraviolet light is shown in figure 1. As shown in fig. 1, the synthesized perovskite quantum dot organic solution emits strong blue, green and red fluorescence respectively under the irradiation of ultraviolet light.
The picture of the synthesized three-color fluorescent perovskite quantum dot under a field emission transmission electron microscope is shown in figure 2. As shown in fig. 2, the perovskite quantum dots are regular cubic nanocrystals with an average diameter of about 9 nm, and have a distinct lattice structure with a lattice spacing of 0.58 nm.
Example 2
The synthesis method of the green perovskite quantum dot functionalized fluorescent paraffin comprises the following steps: 5 g of paraffin wax (melting point 65 ℃) were taken and heated to complete melting. And then adding 0.5 mL of green fluorescent perovskite quantum dot n-hexane solution into the molten paraffin, and uniformly stirring. And (3) in a vacuum drying oven at 65 ℃, removing n-hexane in the paraffin under reduced pressure, and cooling to room temperature to obtain the perovskite quantum dot functionalized green fluorescent paraffin.
The synthesis of blue and red fluorescent perovskite quantum dot functionalized paraffin wax is similar to that described above except that blue and red fluorescent perovskite quantum dots are used instead.
The picture of the synthesized perovskite quantum dot functionalized fluorescent paraffin under the irradiation of white light and ultraviolet light is shown in fig. 3. As shown in fig. 3, the synthesized perovskite quantum dot functionalized fluorescent paraffin emits bright blue, green and red fluorescence under an ultraviolet lamp.
Example 3
The method for preparing the cartoon toy from the perovskite quantum dot functionalized fluorescent paraffin comprises the following steps: taking a proper amount of perovskite quantum dot functionalized fluorescent paraffin with different colors, heating and melting the fluorescent paraffin, then quickly pouring the fluorescent paraffin into a prepared cartoon toy mold, and removing the mold after cooling to obtain the fluorescent paraffin cartoon toy with different colors (as shown in figure 4).
Example 4
The method for preparing the color fluorescent powder from the perovskite quantum dot functionalized fluorescent paraffin comprises the following steps: a spraying bottle is filled with a proper amount of perovskite quantum dot functionalized fluorescent paraffin with a specific color, the fluorescent paraffin is heated and melted, and the paraffin is sprayed on A4 paper when the fluorescent paraffin is hot. And in the spraying process, if the fluorescent paraffin in the spraying bottle is cooled and solidified, the spraying bottle is placed back into the furnace to be heated so that the paraffin is remelted, the paraffin is continuously sprayed onto the paper, and the steps are repeated for multiple times until the fluorescent paraffin in the bottle is completely sprayed. And lightly sweeping the fine paraffin particles (the average particle size is about 100 microns) on the paper into a pile by using a clean brush to obtain the fluorescent paraffin powder. Blue, green and red fluorescent powders can be obtained by using blue, green and red fluorescent perovskite quantum dot functionalized fluorescent paraffin (as shown in figure 5).
Example 5
The method for preparing the color LED bulb from the perovskite quantum dot functionalized paraffin fluorescent powder comprises the following steps: an appropriate amount of the fluorescent powder prepared in example 4 was put into a transparent plastic or glass U-shaped tube, and filled, and then turned over on an ultraviolet LED chip to make blue, green, and red LEDs.
The manufacturing method of the white light LED comprises the following steps: the white fluorescent paraffin powder is prepared from blue, green and red fluorescent powder according to a certain proportion. Then, the white light LED is manufactured according to the method.
As can be seen in fig. 6, these LEDs are capable of emitting intense blue, green, red and white light when energized for operation.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (6)
1. A preparation method of perovskite quantum dot functionalized fluorescent paraffin is characterized by comprising the following steps: the method comprises the following steps:
(1) dispersing the perovskite quantum dots by using an organic solution to prepare a uniformly dispersed perovskite quantum dot organic solution;
(2) melting paraffin into liquid by heating and stirring;
(3) injecting the perovskite quantum dot organic solution obtained in the step (1) into the liquid paraffin obtained in the step (2), and fully stirring and mixing to obtain a uniform perovskite quantum dot-organic solvent-paraffin mixed solution;
(4) removing the organic solvent from the mixed solution obtained in the step (3) under reduced pressure under the condition of maintaining a molten state to obtain a perovskite quantum dot-paraffin solution;
(5) and (4) cooling the perovskite quantum dot-paraffin solution obtained in the step (4) to room temperature to obtain the perovskite quantum dot functionalized fluorescent paraffin.
2. The preparation method of the perovskite quantum dot functionalized fluorescent paraffin wax as claimed in claim 1, which is characterized in that: the perovskite quantum dots are all inorganic or organic and inorganic hybrid perovskite quantum dots, and the fluorescence of the perovskite quantum dots is green, blue, red or a mixed color of more than two colors.
3. The preparation method of the perovskite quantum dot functionalized fluorescent paraffin wax as claimed in claim 1, which is characterized in that: the organic solvent comprises n-hexane.
4. The preparation method of the perovskite quantum dot functionalized fluorescent paraffin wax as claimed in claim 1, which is characterized in that: the paraffin is one or more of low-melting-point paraffin, high-melting-point paraffin, liquid paraffin or paraffin derivatives.
5. A perovskite functionalized fluorescent paraffin prepared according to the method of claim 1.
6. Use of the perovskite functionalized fluorescent paraffin as claimed in claim 5 in the preparation of fluorescent paraffin toys, fluorescent candles, fluorescent crayons, fluorescent waxed paper and fluorescent powder.
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| CN1521214A (en) * | 2003-01-30 | 2004-08-18 | 张钟潜 | Process for preparing luminous wax product |
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| US9577127B1 (en) * | 2015-09-11 | 2017-02-21 | Tianjin Zhonghuan Quantum Tech Co., Ltd. | Composite material for fluorescent quantum dot micro-nano packaging |
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| WO2018049389A1 (en) * | 2016-09-12 | 2018-03-15 | North Carolina State University | Redox catalysts for the oxidative cracking of hydrocarbons, methods of making, and methods of use thereof |
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