CN111676010A - Preparation method of perovskite quantum dot/Eu-MOF composite luminescent material - Google Patents
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Abstract
The invention discloses a preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material, which comprises the following steps: s1, adding europium nitrate hexahydrate and biphenyltetracarboxylic acid into a mixed solution of DMF (dimethyl formamide) and water, heating and cooling, removing residual DMF, and carrying out vacuum drying to obtain an Eu-MOF crystal; s2, mixing the dried Eu-MOF crystals with PbBr2Mixing the obtained DMF solution to obtain PbBr2A precursor solution of @ Eu-MOF; s3, adding CsBr, stirring until the mixture is clear, and adding oleic acid oleylamine; then transferring the mixture to methylbenzene to preliminarily prepare a perovskite quantum dot/Eu-MOF composite luminescent material; s4, the materials are centrifugally dispersed in a normal hexane solution, stirred and filtered to obtain a high-purity perovskite quantum dot/Eu-MOF composite luminescent material, so that the problem of poor stability of perovskite quantum dots and the defect of red light area of the conventional white light LED are solvedThe problem of loss.
Description
Technical Field
The invention relates to the field of composite luminescent materials, in particular to a preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material.
Background
All inorganicPerovskite quantum dot CsPbX3The (X ═ Cl, Br, I) has the advantages of high quantum yield, adjustable luminescence, narrow emission spectrum and wide color gamut, and the like, and shows great potential in the aspect of optoelectronic devices. However, perovskite quantum dots are chemically poorly stable under ambient conditions due to their ionic properties and are very sensitive to humidity, light and temperature. In addition, the high degree of ionization of the internal bonds makes them highly susceptible to ion exchange reactions. How to solve the stability problem of the perovskite quantum dots becomes a difficult problem to be solved urgently.
The MOFs material has the characteristics of porosity, high specific surface area, unsaturated metal sites, structural diversity and the like, so that the MOFs material has some special physical and chemical properties. The magnetic material has attracted extensive attention of researchers in recent years, and has a promising application prospect in a plurality of fields such as gas storage and separation, molecular recognition, photoelectric magnetic material, drug delivery and the like. The MOFs can be used as a host material to receive various guest materials so as to realize the assembly of novel functional materials. As mentioned earlier, perovskite quantum dots are also the focus of research in recent years. Therefore, the combination of the two materials can realize the regulation and the synergistic improvement of the performance, various novel quantum dot @ MOFs composite materials can be produced at once, and the application field of the composite materials is continuously expanded.
At present, a white light LED mainly adopts a device structure of yellow fluorescent powder which can be effectively excited by a blue light chip and blue light, but the structure has obvious defects that a red light component is lacked, and a spectrum does not completely cover a visible light range, so that the formed white light has a low color rendering index. In order to solve the problem of red light deficiency, a great deal of research is carried out on realizing the combined luminescence of the perovskite quantum dots and the rare earth ions by a rare earth ion doping mode, but the mode still has the problem of poor intrinsic stability of the perovskite quantum dots, the doping amount of the rare earth ions is limited, large-dose doping cannot be realized, and the luminescence of the rare earth ions is much weaker than that of the perovskite quantum dots.
Disclosure of Invention
The invention aims to provide a preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material, wherein Eu-MOF is used for stabilizing the perovskite quantum dot, so that the problem of poor stability of the perovskite quantum dot is solved, and the problem of red light area deficiency of the existing white light LED is solved.
In order to achieve the purpose, the technical scheme of the invention is realized as follows:
the invention provides a preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material, which comprises the following steps:
s1, adding europium nitrate hexahydrate and biphenyl tetracarboxylic acid into a mixed solution of DMF (dimethyl formamide) and water, wherein the molar ratio of the europium nitrate hexahydrate to the biphenyl tetracarboxylic acid is 1: 0.2-1;
putting the mixed solution into a reaction kettle, heating to 100 ℃ and 150 ℃, and reacting for 10-48 h; naturally cooling to room temperature, carrying out suction filtration and purification on the product, removing residual DMF, and carrying out vacuum drying to obtain Eu-MOF crystals;
s2, mixing the dried Eu-MOF crystals with PbBr2The DMF solution is mixed and stirred for a certain time to obtain PbBr2A precursor solution of @ Eu-MOF;
s3, in PbBr2Adding CsBr into the precursor solution of @ Eu-MOF, stirring until the solution is clear, and adding oleic acid oleylamine; then transferring the mixture to methylbenzene to preliminarily prepare a perovskite quantum dot/Eu-MOF composite luminescent material;
s4, centrifugally dispersing the perovskite quantum dot/Eu-MOF composite luminescent material preliminarily prepared in the step S3 in a normal hexane solution, uniformly stirring, filtering out precipitates, removing the perovskite quantum dot remaining on the surface, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
Further, the molar ratio of europium nitrate hexahydrate and biphenyltetracarboxylic acid in the step S1 is 1: 0.6.
Further, in step S1, the volume ratio of DMF to water is 5: 0.5-2.
Further, in the step S1, Eu-MOF crystals are prepared by vacuum drying for 5-10h at the temperature of 50-80 ℃.
Further, in the step S2, the volume of the DMF solution is 5-20ml, and Eu-MOF crystals and PbBr are mixed2The DMF solution is stirred for 6 to 24 hours.
Further, in step S2, CsBr and PbBr2Is 1: 1.
Further, in the step S3, CsBr and PbBr are prepared2The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene is (0.1-2): 10.
Furthermore, the perovskite quantum dot/Eu-MOF composite luminescent material prepared by the preparation method is applied to LEDs.
Further, the perovskite quantum dot/Eu-MOF composite luminescent material is mixed with ultraviolet curing glue, the mixture is dripped on a blue light LED chip, and the white light LED is obtained after curing under ultraviolet light.
By adopting the technical scheme, the preparation method of the perovskite quantum dot/Eu-MOF composite luminescent material has the following technical effects:
1) the application adopts MOF to follow PbBr first2A step of mixing is carried out, making it possible to couple the MOF to Pb2+Ions are adsorbed, so that the next-step synthesis of the composite material is facilitated, the perovskite quantum dots and the MOF are better combined, the perovskite quantum dots are better dispersed in the MOF, and the stability of the perovskite quantum dots is improved, and meanwhile, the excellent optical characteristics of the perovskite quantum dots are effectively reserved;
2) by adjusting the components of the perovskite quantum dots, the perovskite quantum dots CsPbX covering the visible light range can be obtained3a/Eu-MOF composite luminescent material;
3) the green luminescence property of the perovskite quantum dots and the red luminescence property of the rare earth MOF are utilized to synthesize a composite luminescent material capable of emitting green light and red light simultaneously, the composite luminescent material solves the problem of the perovskite quantum dots in LED application, and the application of the perovskite quantum dots in the aspect of LEDs is promoted;
4) the method has the advantages of simple raw materials, mild reaction conditions, simple operation and high efficiency.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 shows CsPbBr obtained in example 13A Transmission Electron Microscope (TEM) image of the/Eu-MOF composite luminescent material.
FIG. 2 shows CsPbBr prepared in example 13Emission spectrum of the/Eu-MOF composite luminescent material.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the accompanying drawings, and it should be understood that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The present invention will be described in further detail below with reference to specific embodiments and with reference to the attached drawings.
The application provides a preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material, which comprises the following steps:
s1, adding europium nitrate hexahydrate and biphenyltetracarboxylic acid into an aqueous solution of DMF (N, N-dimethylformamide), wherein the molar ratio of the europium nitrate hexahydrate to the biphenyltetracarboxylic acid is 1: 0.2-1;
putting the mixed solution into a reaction kettle, heating to 100 ℃ and 150 ℃, and reacting for 10-48 h; naturally cooling to room temperature, carrying out suction filtration and purification on the product, removing residual DMF (N, N-dimethylformamide), and carrying out vacuum drying to obtain Eu-MOF crystals;
in the scheme, the Eu-MOF crystal is prepared from the rigid and highly symmetrical biphenyltetracarboxylic acid, so that the Eu-MOF crystal has a more excellent energy transfer effect, and further the MOF material with excellent fluorescence performance is obtained;
s2, mixing the dried Eu-MOF crystals with PbBr2The DMF solution is mixed and stirred for a certain time to obtain PbBr2A precursor solution of @ Eu-MOF;
s3, in PbBr2Adding the precursor solution of @ Eu-MOFCsBr, stirring until the mixture is clear, and adding oleic acid oleylamine; then transferring the mixture to methylbenzene to preliminarily prepare a perovskite quantum dot/Eu-MOF composite luminescent material;
s4, centrifugally dispersing the perovskite quantum dot/Eu-MOF composite luminescent material preliminarily prepared in the step S3 in a normal hexane solution, uniformly stirring, filtering out precipitates, removing the perovskite quantum dot residual on the surface, and drying in vacuum to prepare the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
In a preferred embodiment, the molar ratio of europium nitrate hexahydrate and biphenyltetracarboxylic acid in step S1 is 1: 0.6.
In a preferred embodiment, in step S1, the volume ratio of DMF to water is 5: 0.5-2, and in practice, the volume ratio of DMF to water may be 5: 0.5, 5: 1, or 5: 2.
In a preferred embodiment, in step S1, the Eu-MOF crystals are prepared by vacuum drying at a temperature of 50-80 ℃ for 5-10h, and optionally, the Eu-MOF crystals are prepared by vacuum drying at a temperature of 60 ℃ for 8 h.
In a preferred embodiment, in the step S2, the volume of the DMF solution is 5-20ml, and the Eu-MOF crystals and PbBr are mixed2The DMF solution is stirred for 6 to 24 hours.
In a preferred embodiment, in the step S2, CsBr and PbBr2Is 1: 1.
In a preferred embodiment, in the step S3, the prepared CsBr and PbBr are2The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene is (0.1-2):10, for example, CsBr and PbBr when applied2The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene can be 0.1: 10,1: 10, or 2: 10 to equal proportions.
The preparation method of the perovskite quantum dot/Eu-MOF composite luminescent material provided by the application comprises the following steps:
the used solvothermal method is synthesized at room temperature, and the preparation can be carried out at room temperature without any inert atmosphere protection, so that the preparation method has the advantage of simplicity;
process for compositing perovskite quantum dots and MOFsIn the application, MOF is firstly mixed with PbBr2A step of mixing is carried out, which makes it possible to couple the MOF to Pb2+Ions are adsorbed, so that the synthesis of the composite material in the next step is facilitated, the perovskite quantum dots and the MOF are better combined, and the perovskite quantum dots are better in dispersibility in the MOF;
in addition, a composite luminescent material capable of simultaneously emitting green light and red light is synthesized by utilizing the green luminescence property of the perovskite quantum dots and the red luminescence property of the rare earth MOF, and the rare earth MOF plays a role in protecting the perovskite quantum dots.
The production method of the present application will be described below with reference to specific examples.
Example 1
Weighing 1.784g (4mmol) of Eu (NO)3)3·6H2O, 0.6605g (2mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring2In O solution;
then placing the mixed solution into a teflon autoclave lining with the volume of 50ml, and heating for 48 hours in the environment of the temperature of 120 ℃; after cooling, the powder obtained is filtered off and washed with DMF and then with chloroform solution to remove residual DMF;
and (3) drying the obtained product at 80 ℃ for 2 hours in vacuum to obtain Eu-MOF crystals.
Mixing 0.4g of the above Eu-MOF crystal after drying with 0.1468g of PbBr2Mixing and stirring the mixture in 10ml of DMF solution for a period of time to obtain PbBr2A precursor solution of @ Eu-MOF;
then to PbBr2Adding 0.085g CsBr solution into the precursor solution of @ Eu-MOF, stirring until the solution is clear, and adding 1ml of oleic acid and 0.5ml of oleylamine;
1ml of the prepared solution is transferred to 10ml of toluene solution to obtain a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and performing centrifugal precipitation and dispersion on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material in a normal hexane solution at 8000-10000r/min, then performing centrifugal filtration to obtain precipitate, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
Example 2
Weighing 1.784g (4mmol) of Eu (NO)3)3·6H2O, 0.6605g (2mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring2In O solution;
then placing the mixed solution into a teflon autoclave lining with the volume of 50ml, and heating for 48 hours in the environment of 100 ℃; after cooling, the powder obtained is filtered off and washed with DMF and then with chloroform solution to remove residual DMF;
and (3) drying the obtained product at 80 ℃ for 2 hours in vacuum to obtain Eu-MOF crystals.
Mixing 0.4g of the above Eu-MOF crystal after drying with 0.1468g of PbBr2Mixing and stirring the mixture in 10ml of DMF solution for a period of time to obtain PbBr2A precursor solution of @ Eu-MOF;
then to PbBr2Adding 0.085g CsBr solution into the precursor solution of @ Eu-MOF, stirring until the solution is clear, and adding 1ml of oleic acid and 0.5ml of oleylamine;
1ml of the prepared solution is transferred to 10ml of toluene solution to obtain a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and performing centrifugal precipitation and dispersion on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material in a normal hexane solution at 8000-10000r/min, then performing centrifugal filtration to obtain precipitate, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
Example 3
Weighing 1.784g (4mmol) of Eu (NO)3)3·6H2O, 0.6605g (2mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring2In O solution;
then placing the mixed solution into a teflon autoclave lining with the volume of 50ml, and heating for 48 hours in the environment of the temperature of 120 ℃; after cooling, the powder obtained is filtered off and washed with DMF and then with chloroform solution to remove residual DMF;
and (3) drying the obtained product at 80 ℃ for 2 hours in vacuum to obtain Eu-MOF crystals.
Mixing 0.4g of the above Eu-MOF crystals after drying with 0.28g of PbBr2Mixing and stirring the mixture in 10ml of DMF solution for a period of time to obtain PbBr2A precursor solution of @ Eu-MOF;
then to PbBr2Adding 0.16g CsBr solution into the precursor solution of @ Eu-MOF, stirring until the solution is clear, and adding 1ml of oleic acid and 0.5ml of oleylamine;
1ml of the prepared solution is transferred to 10ml of toluene solution to obtain a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and performing centrifugal precipitation and dispersion on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material in a normal hexane solution at 8000-10000r/min, then performing centrifugal filtration to obtain precipitate, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
As shown in FIG. 1, CsPbBr was prepared for example 13A Transmission Electron Microscope (TEM) image of the/Eu-MOF composite luminescent material. As can be seen from FIG. 1, CsPbBr3Successfully compounded with Eu-MOF.
Perovskite Quantum dot CsPbBr prepared in example 13The emission spectrum of the/Eu-MOF composite luminescent material is shown in FIG. 2, and CsPbBr can be seen from the graph3The Eu-MOF composite luminescent material realizes the combined luminescence of green light and red light.
In addition, the embodiment of the application also provides a perovskite quantum dot/Eu-MOF composite luminescent material, the composite luminescent material is prepared by the preparation method, and the composite luminescent material can be applied to LEDs.
Preferably, in specific application, the perovskite quantum dot/Eu-MOF composite luminescent material is mixed with ultraviolet curing glue, the mixture is dripped on a blue LED chip, and the white LED is obtained after curing under ultraviolet light.
It should be noted that, the current mainstream white light LED adopts a combination mode of blue light and yellow light, so that a red light part is lacked3Perovskite quantum dots and red emitting rare earth EUThe MOF is combined into a composite luminescent material, and then is combined with a blue light chip to obtain a white light LED; and Eu-MOF can also play a role in protecting the perovskite quantum dots.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (9)
1. A preparation method of a perovskite quantum dot/Eu-MOF composite luminescent material is characterized by comprising the following steps:
s1, adding europium nitrate hexahydrate and biphenyl tetracarboxylic acid into a mixed solution of DMF (dimethyl formamide) and water, wherein the molar ratio of the europium nitrate hexahydrate to the biphenyl tetracarboxylic acid is 1: 0.2-1;
putting the mixed solution into a reaction kettle, heating to 100 ℃ and 150 ℃, and reacting for 10-48 h; naturally cooling to room temperature, carrying out suction filtration and purification on the product, removing residual DMF, and carrying out vacuum drying to obtain Eu-MOF crystals;
s2, mixing the dried Eu-MOF crystals with PbBr2The DMF solution is mixed and stirred for a certain time to obtain PbBr2A precursor solution of @ Eu-MOF;
s3, in PbBr2Adding CsBr into the precursor solution of @ Eu-MOF, stirring until the solution is clear, and adding oleic acid oleylamine; then transferring the mixture to methylbenzene to preliminarily prepare a perovskite quantum dot/Eu-MOF composite luminescent material;
s4, centrifugally dispersing the perovskite quantum dot/Eu-MOF composite luminescent material preliminarily prepared in the step S3 in a normal hexane solution, uniformly stirring, filtering out precipitates, removing the perovskite quantum dot remaining on the surface, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
2. The method of claim 1, wherein the molar ratio of europium nitrate hexahydrate to biphenyltetracarboxylic acid in step S1 is 1: 0.6.
3. The method of claim 1, wherein in step S1, the volume ratio of DMF to water is 5: 0.5-2.
4. The method of claim 1, wherein in step S1, Eu-MOF crystals are vacuum dried at 50-80 ℃ for 5-10 h.
5. The method of claim 1, wherein in step S2, the volume of the DMF solution is 5-20ml, and the Eu-MOF crystals and PbBr are mixed2The DMF solution is stirred for 6 to 24 hours.
6. The method according to claim 1, wherein in step S2, CsBr and PbBr2Is 1: 1.
7. The method of claim 1, wherein the CsBr and PbBr are prepared in step S32The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene is (0.1-2): 10.
8. The preparation method of any one of claims 1 to 7, wherein the perovskite quantum dot/Eu-MOF composite luminescent material prepared by the preparation method is applied to an LED.
9. The preparation method of claim 8, wherein the perovskite quantum dot/Eu-MOF composite luminescent material is mixed with ultraviolet curing glue, and is dripped on a blue LED chip, and after curing under ultraviolet light, a white LED is obtained.
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| CN113201326A (en) * | 2021-04-22 | 2021-08-03 | 浙江大学 | Dye/perovskite quantum dot loaded metal-organic framework material and preparation method thereof |
| CN113621368A (en) * | 2021-07-20 | 2021-11-09 | 上海大学 | Lead-cesium-halide perovskite quantum dot and metal organic framework compounded moulding ultrafast scintillator and preparation method thereof |
| CN116162456A (en) * | 2023-02-21 | 2023-05-26 | 山东大学 | Preparation method of narrow-band green fluorescent powder of cesium lead bromine perovskite quantum dot embedded metal organic framework material ZIF-8 |
| CN116162456B (en) * | 2023-02-21 | 2024-05-24 | 山东大学 | Preparation method of narrow-band green fluorescent powder of cesium lead bromine perovskite quantum dot embedded metal organic framework material ZIF-8 |
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