CN111676010B - Preparation method of perovskite quantum dot/Eu-MOF composite luminescent material - Google Patents
Preparation method of perovskite quantum dot/Eu-MOF composite luminescent material Download PDFInfo
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Abstract
The invention discloses a perovskite quantumThe preparation method of the dot/Eu-MOF composite luminescent material comprises the following steps: s1, adding europium nitrate hexahydrate and biphenyl tetracarboxylic acid into a mixed solution of DMF and water, heating and cooling, removing residual DMF, and vacuum drying to obtain Eu-MOF crystals; s2, mixing the dried Eu-MOF crystal with PbBr 2 Is mixed with DMF solution to obtain PbBr 2 Precursor solution of @ Eu-MOF; s3, adding CsBr, stirring until the mixture is clear, and adding oleylamine oleate; transferring the mixture into toluene to prepare a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily; s4, centrifugally dispersing the material in a normal hexane solution, stirring, filtering out precipitate and the like to prepare the perovskite quantum dot/Eu-MOF composite luminescent material with high purity, and solving the problem of poor stability of the perovskite quantum dot and the problem of red light region deficiency of the existing white light LED.
Description
Technical Field
The invention relates to the field of composite luminescent materials, in particular to a preparation method of perovskite quantum dot/Eu-MOF composite luminescent materials.
Background
All-inorganic perovskite quantum dot CsPbX 3 (x=cl, br, I) has the advantages of high quantum yield, tunable luminescence, narrow emission spectrum, wide color gamut, and the like, and shows great potential in the aspect of optoelectronic devices. However, perovskite quantum dots are very sensitive to humidity, light and temperature due to their ionic nature, poor chemical stability under ambient conditions. In addition, the high ionization of the internal bonds makes it extremely susceptible to ion exchange reactions. How to solve the stability problem of perovskite quantum dots becomes a difficult problem to be solved urgently.
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 special physical and chemical properties. In recent years, researchers have received extensive attention, and the method has shown application prospects in various fields such as gas storage and separation, molecular recognition, photoelectromagnetic materials, drug delivery and the like. MOFs can accept a variety of guest materials as host materials to achieve the assembly of novel functional materials. As mentioned above, perovskite quantum dots have also been the focus of research in recent years. Therefore, the combination of the two materials can realize the regulation and the cooperative promotion of the performance, and various novel quantum dot MOFs composite materials are generated, so that the application field is also continuously expanded.
At present, a white light LED is mainly a device structure of yellow fluorescent powder which is effectively excited by a blue light chip and blue light energy, but the structure has obvious defects of lacking a red light component and not fully covering a visible light range, so that the color rendering index of the formed white light is lower. 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 in a rare earth ion doping mode, but the problem that the perovskite quantum dots are poor in intrinsic stability is unavoidable in the mode, 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, which uses Eu-MOF to stabilize perovskite quantum dots, solves the problem of poor stability of the perovskite quantum dots, and solves the problem of red light region deficiency existing in the existing white light LED.
In order to achieve the above 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 and water, wherein the molar ratio of the europium nitrate hexahydrate to the biphenyl tetracarboxylic acid is 1: (0.2-1);
the mixed solution is put into a reaction kettle and heated to 100-150 ℃ for reaction for 10-48h; naturally cooling to room temperature, filtering and purifying the resultant, removing residual DMF, and drying in vacuum to obtain Eu-MOF crystals;
s2, mixing the dried Eu-MOF crystal with PbBr 2 After a certain time of mixing and stirring DMF solution of (B) to obtain PbBr 2 Precursor solution of @ Eu-MOF;
s3, at PbBr 2 Adding CsBr into the precursor solution of the @ Eu-MOF, stirring until the mixture is clear, and adding oleylamine oleate; then transferred to toluene for the first timePreparing 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 normal hexane solution, uniformly stirring, filtering out precipitate, removing the perovskite quantum dot remained on the surface, and vacuum drying to prepare the perovskite quantum dot/Eu-MOF composite luminescent material with high purity.
Further, the molar ratio of europium nitrate hexahydrate to biphenyl tetracarboxylic acid in the step S1 is 1:0.6.
Further, in the step S1, the volume ratio of DMF to water is 5: (0.5-2).
Further, in the step S1, the Eu-MOF crystal is dried in vacuum at a temperature of 50-80 ℃ for 5-10 hours.
Further, in the step S2, the volume of the DMF solution is 5-20ml, and the Eu-MOF crystal and PbBr 2 The DMF solution of (C) was stirred for 6-24h.
Further, in the step S2, csBr and PbBr 2 The molar ratio of (2) is 1:1.
Further, in the step S3, csBr and PbBr are prepared 2 The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene is (0.1-2): 10.
Further, the perovskite quantum dot/Eu-MOF composite luminescent material prepared by the preparation method is applied to LEDs.
Further, mixing the perovskite quantum dot/Eu-MOF composite luminescent material with ultraviolet curing glue, dripping the mixture onto a blue light LED chip, and curing the mixture under ultraviolet light to obtain the white light LED.
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 followed by PbBr 2 A step of mixing, the MOF can be made to correspond to Pb 2+ Ions are adsorbed, so that the next step of composite material synthesis is facilitated, the perovskite quantum dots and the MOF are better combined, the perovskite quantum dots have better dispersibility in the MOF, and the perovskite quantum dots are effectively reserved while the stability of the perovskite quantum dots is improvedExcellent mineral quantum dot is a combination of the optical characteristics of (a) and (b);
2) By adjusting the components of the perovskite quantum dots, the perovskite quantum dots CsPbX covering the visible light range can be obtained 3 Eu-MOF composite luminescent material;
3) By utilizing the green luminescence property of the perovskite quantum dots and the red luminescence property of the rare earth MOF, a composite luminescent material capable of simultaneously emitting green light and red light is synthesized, and the composite luminescent material solves the problem of the perovskite quantum dots in LED application, so that the application of the perovskite quantum dots in the LED is promoted;
4) The method has the advantages of simple raw materials, mild reaction conditions, simple operation and high efficiency.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
FIG. 1 is CsPbBr obtained in example 1 3 Transmission Electron Microscope (TEM) image of the Eu-MOF composite luminescent material.
FIG. 2 is CsPbBr obtained in example 1 3 Emission spectrum of Eu-MOF composite luminescent material.
Detailed Description
The following description of the embodiments of the present invention will be made apparent and fully in view of the accompanying drawings, in which some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention will now be described in further detail with reference to specific examples thereof in connection with the accompanying drawings.
The preparation method of the perovskite quantum dot/Eu-MOF composite luminescent material provided by the application comprises the following steps:
s1, adding europium nitrate hexahydrate and biphenyl tetracarboxylic acid into an aqueous solution of DMF (N, N-dimethylformamide), wherein the molar ratio of the europium nitrate hexahydrate to the biphenyl tetracarboxylic acid is 1: (0.2-1);
the mixed solution is put into a reaction kettle and heated to 100-150 ℃ for reaction for 10-48h; naturally cooling to room temperature, filtering and purifying the resultant, removing residual DMF (N, N-dimethylformamide), and drying in vacuum to obtain Eu-MOF crystals;
in the scheme, the biphenyl tetracarboxylic acid with rigidity and high symmetry is used for preparing the Eu-MOF crystal, so that the Eu-MOF crystal has more excellent energy transmission effect, and further the MOF material with excellent fluorescence performance is obtained;
s2, mixing the dried Eu-MOF crystal with PbBr 2 After a certain time of mixing and stirring DMF solution of (B) to obtain PbBr 2 Precursor solution of @ Eu-MOF;
s3, at PbBr 2 Adding CsBr into the precursor solution of the @ Eu-MOF, stirring until the mixture is clear, and adding oleylamine oleate; transferring the mixture into toluene to prepare a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
s4, centrifugally dispersing the perovskite quantum dot/Eu-MOF composite luminescent material preliminarily prepared in the step S3 in normal hexane solution, uniformly stirring, filtering out precipitate, removing the perovskite quantum dot remained on the surface, and vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
In a preferred embodiment, the molar ratio of europium nitrate hexahydrate to biphenyl tetracarboxylic acid in step S1 is 1:0.6.
In a preferred embodiment, in the step S1, the volume ratio of DMF to water is 5:0.5-2, and in practical application, 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 crystal is vacuum dried at a temperature of 50-80℃for 5-10 hours, optionally, the Eu-MOF crystal is vacuum dried at a temperature of 60℃for 8 hours.
In a preferred embodiment, in step S2The volume of DMF solution is 5-20ml, eu-MOF crystal and PbBr 2 The DMF solution of (C) was stirred for 6-24h.
In a preferred embodiment, in step S2, csBr and PbBr 2 The molar ratio of (2) is 1:1.
In a preferred embodiment, in the step S3, csBr and PbBr are prepared 2 The volume ratio of mixed precursor solution of @ Eu-MOF to toluene is (0.1-2): 10, e.g., csBr and PbBr when applied 2 The volume ratio of mixed precursor solution of @ Eu-MOF to toluene may be 0.1:10,1:10, or 2:10, equal proportions.
The preparation method of the perovskite quantum dot/Eu-MOF composite luminescent material provided by the application comprises the following steps:
the method uses solvothermal method to synthesize at room temperature, can prepare at room temperature without any inert atmosphere protection, and has the advantage of simple preparation method;
in the process of compositing perovskite quantum dots and MOFs, the application adopts MOFs and PbBr firstly 2 A step of mixing which can make MOF to Pb 2+ Ions are adsorbed, so that the next step of composite material synthesis is facilitated, perovskite quantum dots and MOFs are better combined, and the perovskite quantum dots have better dispersibility in the MOFs;
in addition, 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 simultaneously emitting green light and red light, and the rare earth MOF plays a role in protecting the perovskite quantum dots.
The preparation method of the present application will be described with reference to specific examples.
Example 1
1.784g (4 mmol) of Eu (NO) was weighed out 3 ) 3 ·6H 2 O, 0.6605g (2 mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring 2 O solution;
then the mixed solution is placed in a Teflon autoclave liner with the volume of 50ml and heated for 48 hours in the temperature environment of 120 ℃; after cooling, the resulting powder was filtered off and washed with DMF, then with chloroform solution to remove residual DMF;
the obtained product was vacuum-dried at 80℃for 2 hours to obtain Eu-MOF crystals.
Drying 0.4g and 0.1468g of PbBr of the Eu-MOF crystal 2 Mixing and stirring in 10ml DMF solution for a period of time to obtain PbBr 2 Precursor solution of @ Eu-MOF;
and then to PbBr 2 Adding 0.085g of 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;
transferring 1ml of the prepared solution into 10ml of toluene solution to obtain perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and (3) performing centrifugal precipitation on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material at 8000-10000r/min, dispersing in normal hexane solution, performing centrifugal filtration to precipitate, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
Example 2
1.784g (4 mmol) of Eu (NO) was weighed out 3 ) 3 ·6H 2 O, 0.6605g (2 mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring 2 O solution;
then the mixed solution is placed in a Teflon autoclave liner with the volume of 50ml and heated for 48 hours in a temperature environment of 100 ℃; after cooling, the resulting powder was filtered off and washed with DMF, then with chloroform solution to remove residual DMF;
the obtained product was vacuum-dried at 80℃for 2 hours to obtain Eu-MOF crystals.
Drying 0.4g and 0.1468g of PbBr of the Eu-MOF crystal 2 Mixing and stirring in 10ml DMF solution for a period of time to obtain PbBr 2 Precursor solution of @ Eu-MOF;
and then to PbBr 2 Adding 0.085g of 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;
transferring 1ml of the prepared solution into 10ml of toluene solution to obtain perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and (3) performing centrifugal precipitation on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material at 8000-10000r/min, dispersing in normal hexane solution, performing centrifugal filtration to precipitate, and performing vacuum drying to obtain the high-purity perovskite quantum dot/Eu-MOF composite luminescent material.
Example 3
1.784g (4 mmol) of Eu (NO) was weighed out 3 ) 3 ·6H 2 O, 0.6605g (2 mmol) of biphenyltetracarboxylic acid, 7.5ml of N, N-Dimethylformamide (DMF) and 2.5ml of H were added with stirring 2 O solution;
then the mixed solution is placed in a Teflon autoclave liner with the volume of 50ml and heated for 48 hours in the temperature environment of 120 ℃; after cooling, the resulting powder was filtered off and washed with DMF, then with chloroform solution to remove residual DMF;
the obtained product was vacuum-dried at 80℃for 2 hours to obtain Eu-MOF crystals.
0.4g and 0.28g of PbBr of the Eu-MOF crystal after drying 2 Mixing and stirring in 10ml DMF solution for a period of time to obtain PbBr 2 Precursor solution of @ Eu-MOF;
and then to PbBr 2 Adding 0.16g of 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;
transferring 1ml of the prepared solution into 10ml of toluene solution to obtain perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
and (3) performing centrifugal precipitation on the primarily prepared perovskite quantum dot/Eu-MOF composite luminescent material at 8000-10000r/min, dispersing in normal hexane solution, performing centrifugal filtration to 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 in example 1 3 Transmission Electron Microscope (TEM) image of the Eu-MOF composite luminescent material. As can be seen from FIG. 1, csPbBr 3 Compounding with Eu-MOF successfully.
Perovskite quantum dot CsPbBr prepared in example 1 3 The emission spectrum of the Eu-MOF composite luminescent material is shown in FIG. 2, and CsPbBr can be seen from the graph 3 The 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, which is prepared by the preparation method and can be applied to LEDs.
Preferably, in specific application, the perovskite quantum dot/Eu-MOF composite luminescent material is mixed with ultraviolet curing glue and is dripped on a blue light LED chip, and after curing under ultraviolet light, the white light LED is obtained.
It should be noted that, the current mainstream white light LED adopts a combination of blue light and yellow light, so that the red light portion is lacking, and the technical scheme of the application is to use CsPbBr emitting green light 3 The perovskite quantum dots and the rare earth EU-MOF emitting red light form a composite luminescent material, and then the composite luminescent material is combined with a blue light chip to obtain a white light LED; and Eu-MOF can also play a role in protecting perovskite quantum dots.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (9)
1. The preparation method of the 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 and water, wherein the molar ratio of the europium nitrate hexahydrate to the biphenyl tetracarboxylic acid is 1: (0.2-1);
the mixed solution is put into a reaction kettle and heated to 100-150 ℃ for reaction for 10-48h; naturally cooling to room temperature, filtering and purifying the resultant, removing residual DMF, and drying in vacuum to obtain Eu-MOF crystals;
s2, mixing the dried Eu-MOF crystal with PbBr 2 After a certain time of mixing and stirring DMF solution of (B) to obtain PbBr 2 Precursor solution of @ Eu-MOF;
s3, at PbBr 2 Adding CsBr into the precursor solution of the @ Eu-MOF, stirring until the mixture is clear, and adding oleylamine oleate; transferring the mixture into toluene to prepare a perovskite quantum dot/Eu-MOF composite luminescent material preliminarily;
s4, centrifugally dispersing the perovskite quantum dot/Eu-MOF composite luminescent material preliminarily prepared in the step S3 in normal hexane solution, uniformly stirring, filtering out the precipitate, removing the perovskite quantum dots remained on the surface, and vacuum drying to obtain the perovskite quantum dot/Eu-MOF composite luminescent material with high purity.
2. The method of claim 1, wherein the europium nitrate hexahydrate and the biphenyltetracarboxylic acid in step S1 are present in a molar ratio of 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, the Eu-MOF crystal is dried in vacuum at a temperature of 50 to 80℃for 5 to 10 hours.
5. The method of claim 1, wherein in step S2, the DMF solution has a volume of 5 to 20ml, and the Eu-MOF crystals and PbBr 2 The DMF solution of (C) was stirred for 6-24h.
6. The method of claim 1, wherein in steps S2 to S3, csBr and PbBr are mixed 2 The molar ratio of (2) is 1:1.
7. Such asThe process according to claim 1, wherein in step S3, csBr and PbBr are prepared 2 The volume ratio of the mixed precursor solution of @ Eu-MOF to toluene is (0.1-2): 10.
8. Use of the perovskite quantum dot/Eu-MOF composite luminescent material prepared by the method of any one of claims 1-7 in LEDs.
9. The use according to 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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