CN113755167B - Lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder and preparation method and application thereof - Google Patents
Lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nano crystal fluorescent powder, which comprises the following steps: s1, adding metal halide PbX 2 Adding mandelic acid and oleylamine into the octadecylene solution, and stirring for 0.5-5 h at the temperature of 60-160 ℃ to obtain a solution of Pb-mandelic acid organic complex; s2, adding an oleic acid solution of cesium carbonate into a solution of a Pb-mandelic acid organic complex, reacting for 3 s-30 min at 80-180 ℃ in an inert atmosphere, and performing post-treatment to obtain inorganic lead halide perovskite nanocrystalline fluorescent powder coated by a lead organic complex; metal halide PbX 2 The molar ratio to mandelic acid was 1: (0.5 to 5); implanting cesium ions with metal halide PbX 2 The molar ratio of (0.5-2): 1. the fluorescent powder has good fluorescence performance, can be stably stored in an air environment, has the fluorescence quantum efficiency of about 48 percent, has the emission peak position of 519nm and the half-peak width of about 17nm, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of synthesis of photoelectric materials and nano materials, in particular to lead organic complex coated all-inorganic lead halogen perovskite nano crystal fluorescent powder and a preparation method and application thereof.
Background
Due to the advantages of high fluorescence quantum yield, narrow fluorescence emission, wide color gamut and the like, the all-inorganic lead-containing perovskite nano-crystal causes extensive research of researchers, but the existing all-inorganic lead-containing perovskite nano-crystal has the problem of poor stability and limits the wide application of the nano-crystal.
The invention Chinese patent CN110872510A discloses a method for synthesizing perovskite nanocrystalline fluorescent powder by a thermal injection method, which improves the stability of the nanocrystalline fluorescent powder by coating a silicon dioxide shell on the surface of the nanocrystalline fluorescent powder, but the nanocrystalline fluorescent powder prepared by the method can generate obvious fluorescent peak position shift after coating, and the controllable synthesis of the peak position cannot be realized.
Disclosure of Invention
The invention aims to overcome the problems that the fluorescent peak position of the nanocrystalline fluorescent powder prepared by the prior art is deviated and the controllable synthesis of the peak position cannot be realized, and provides a preparation method of the lead-organic complex-coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder.
The invention also aims to provide the lead-organic complex-coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder.
The invention further aims to provide application of the lead-organic complex coated all-inorganic lead-halogen perovskite nano-crystalline fluorescent powder.
The above purpose of the invention is realized by the following technical scheme:
a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder comprises the following steps:
s1, adding metal halide PbX 2 Adding mandelic acid and oleylamine into the octadecene solution, and stirring for 0.5-5 h at the temperature of 60-160 ℃ to obtain a solution of a Pb-mandelic acid organic complex;
s2, adding an oleic acid solution of cesium carbonate into a solution of a Pb-mandelic acid organic complex, reacting for 3 s-30 min at 80-180 ℃ in an inert atmosphere, and performing post-treatment to obtain inorganic lead halide perovskite nanocrystalline fluorescent powder coated by a lead organic complex;
the metal halide PbX 2 The molar ratio to mandelic acid was 1: (0.5 to 5);
cesium ions and metal halide PbX in the oleic acid solution of cesium carbonate 2 In a molar ratio of (0.5-2): 1.
the invention is realized by adding metal halide PbX 2 Adding Mandelic Acid (MA) and oleylamine into octadecene to obtain solution of Pb-mandelic acid organic complex, and further treating with carbonic acidAfter introducing a Cs source into an oleic acid solution of cesium, in-situ synthesis is carried out on the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder, so that the problem of fluorescence peak position shift caused by coating a quantum dot obtained by preparation firstly is solved.
The lead organic complex provides an effective space structure framework for the perovskite nanocrystalline, so that the nanocrystalline can be uniformly dispersed in the lead organic complex without agglomeration, fluorescence quenching is effectively avoided, and the nanocrystalline can keep good fluorescence performance under powder. Meanwhile, the lead organic complex has good stability, the stability of the composite material is also ensured, so that the all-inorganic perovskite nanocrystalline fluorescent powder of the lead organic complex can stably exist in an air environment, and the lead organic complex has good water stability.
The metal halide PbX of the invention 2 Selected from PbCl 2 、PbBr 2 、PbI 2 One or more of (a).
Octadecene solutions of concentrations conventional in the art may be used in the present invention. Preferably, the concentration of the octadecene solution is 90%.
Preferably, the oleylamine is an oleylamine solution, and the concentration of the oleylamine solution is 70% to 98%.
The mandelic acid is selected from one or more of DL-mandelic acid, D-mandelic acid and L-mandelic acid. Preferably, the mandelic acid is DL-mandelic acid.
The post-treatment of the invention comprises cooling, stirring, centrifuging, cleaning and drying in sequence. The cooling is preferably ice-water bath cooling, and the stirring time is 10 min-5 h.
Preferably, the metal halide PbX 2 The molar ratio to mandelic acid was 1: (0.8-2).
More preferably, the metal halide PbX 2 The molar ratio to mandelic acid was 1:1.
preferably, cesium ions in an oleic acid solution of cesium carbonate are combined with a metal halide PbX 2 Molar ratio (0.8 to 1.2): 1.
preferably, the stirring temperature is 120-160 ℃ and the stirring time is 0.5-2 h.
Preferably, the reaction temperature is 140-160 ℃ and the reaction time is 3-60 s.
The lead organic complex coated inorganic lead halogen perovskite nano crystal fluorescent powder is prepared by the method.
The invention also protects the application of the lead organic complex coated all-inorganic lead halogen perovskite nano crystal fluorescent powder in the display field.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder, which is characterized in that the method synthesizes the lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder in situ, thereby overcoming the problem of fluorescence peak position shift caused by coating a quantum dot after preparing the quantum dot. The all-inorganic perovskite fluorescent powder has good fluorescence performance, can be stably stored in an air environment, has the fluorescence quantum efficiency of about 48 percent, has the emission peak position of 519nm and the half-peak width of about 17nm, is easy to store, and has wide application prospect in the field of high-performance display.
Drawings
Fig. 1 is an SEM image of the lead organic complex-coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1.
Fig. 2 is an XRD pattern of the lead organic complex prepared in example 1.
Fig. 3 is an XRD pattern of the lead-organic complex coated all-inorganic lead-halogen perovskite nano-crystalline phosphor prepared in example 1.
Fig. 4 is a photoluminescence chart of the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1.
FIG. 5 is a graph showing the change of fluorescence intensity of the lead-organic complex-coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1 with the time of soaking in water.
Fig. 6 is an electroluminescence diagram of LED devices prepared from the lead-organic complex-coated all-inorganic lead-halogen perovskite nanocrystalline phosphor and blue light chips and commercial red powder prepared in example 1.
Fig. 7 is a graph of the fluorescence quantum yield of the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
Example 1
A preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder comprises the following steps:
s1, adding 0.4mmol of PbBr 2 Adding 0.4mmol of DL-mandelic acid and 1.0mL of oleylamine with the concentration of 70% into 10mL of octadecene solution with the concentration of 90%, heating to 120 ℃, and stirring for 1h to obtain a solution of a Pb-MA organic complex;
s2, injecting 0.8mL of an oleic acid solution of cesium carbonate into the solution of the Pb-MA organic complex, reacting for 10s at 160 ℃ in a nitrogen atmosphere, cooling in an ice water bath, stirring for 1h, centrifuging the reaction solution, pouring out the supernatant, washing with methyl acetate and cyclohexane once respectively, and drying the precipitate to obtain the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder coated by the lead organic complex.
Example 2
Unlike example 1, the amount of DL-mandelic acid in this example was changed to 0.2mmol.
Example 3
Unlike example 1, the amount of DL-mandelic acid was changed to 0.32mmol.
Example 4
Unlike example 1, the amount of DL-mandelic acid was changed to 0.8mmol.
Example 5
Unlike example 1, the amount of DL-mandelic acid was changed to 2.0mmol.
Example 6
Unlike example 1, the cesium ion concentration in the oleic acid solution of cesium carbonate was 0.4mmol/mL.
Example 7
Unlike example 1, the cesium ion concentration in the oleic acid solution of cesium carbonate was 0.6mmol/mL.
Example 8
Unlike example 1, the cesium ion concentration in the oleic acid solution of cesium carbonate was 0.25mmol/mL.
Example 9
Unlike example 1, the cesium ion concentration in the oleic acid solution of cesium carbonate was 1.0mmol/mL.
Example 10
The embodiment provides a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder, which comprises the following steps:
s1, adding 0.4mmol of PbCl 2 Adding 0.4mmol of D-mandelic acid and 2.0mL of oleylamine with the concentration of 70% into 10mL of octadecene solution with the concentration of 90%, heating to 60 ℃, and stirring for 5 hours to obtain a solution of a Pb-MA organic complex;
s2, injecting 0.8mL of an oleic acid solution of cesium carbonate into the solution of the Pb-MA organic complex, reacting for 30min at 80 ℃ in a nitrogen atmosphere, cooling in an ice water bath, stirring for 1h, centrifuging the reaction solution, pouring out the supernatant, washing with methyl acetate and cyclohexane once respectively, and drying the precipitate to obtain the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder coated by the lead organic complex.
Example 11
The embodiment provides a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder, which comprises the following steps:
s1, adding 0.4mmol of PbI 2 Adding 0.4mmol L-mandelic acid and 0.2mL 98% oleylamine into 10mL 90% octadecene solution, heating to 160 deg.C, and stirring for 0.5h to obtain Pb-MA organic complex solution;
s2, injecting 0.8mL of an oleic acid solution of cesium carbonate into a solution of a Pb-MA organic complex, reacting for 3s at 180 ℃ in a nitrogen atmosphere for 1h after cooling in an ice water bath, stirring for 1h, centrifuging the reaction solution, pouring out a supernatant, washing with methyl acetate and cyclohexane once respectively, and drying the precipitate to obtain the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder coated by the lead organic complex.
Example 12
The embodiment provides a preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder, which comprises the following steps:
s1, adding 0.4mmol of PbBr 2 Adding 0.4mmol of DL-mandelic acid and 1.0mL of oleylamine with the concentration of 70% into 10mL of octadecene solution with the concentration of 90%, heating to 120 ℃, and stirring for 0.5h to obtain a solution of a Pb-MA organic complex;
s2, injecting 0.8mL of an oleic acid solution of cesium carbonate into the solution of the Pb-MA organic complex, reacting for 3s at 160 ℃ in a nitrogen atmosphere, cooling in an ice water bath, stirring for 1h, centrifuging the reaction solution, pouring out the supernatant, washing with methyl acetate and cyclohexane once respectively, and drying the precipitate to obtain the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder coated by the lead organic complex.
Comparative example 1
The comparative example provides a preparation process of a green perovskite quantum dot stable fluorescent powder based on silicon dioxide coating, and the preparation process specifically comprises the following steps:
s1, accurately weighing 0.407g of cesium carbonate, 1.5mL of oleic acid and 20mL of octadecene, and adding the cesium carbonate and the oleic acid into a two-neck round-bottom flask. Heating to 130 deg.C under vacuum condition, maintaining for 1h, cooling to 100 deg.C, and introducing nitrogen;
s2, accurately weighing PbBr 2 0.276g, weighing 20mL of octadecene, 2mL of oleic acid and 2mL of oleylamine, adding into a 100mL three-neck round-bottom flask, heating to 120 ℃ in a vacuum state, keeping for 1h, introducing nitrogen, and rapidly heating to 180 ℃;
s3, sucking cesium oleate precursor by using an injector1.6mL of the solution was rapidly injected into PbBr 2 In the precursor solution, after 5s, rapidly cooling to room temperature in an ice-water bath;
s4, centrifuging the liquid product at 5000rpm to obtain a precipitate, adding 5mL of n-hexane, centrifuging at 5000rpm again, and taking a supernatant;
s5, adding 100 mu L of APTES into the clear liquid, stirring at room temperature for 20min, taking the precipitate, cleaning in n-hexane for 3 times, and naturally airing for 20min to obtain a final product.
The photoluminescence spectrum of the product prepared by the comparative example refers to patent CN110872510A and attached figure 1. The fluorescence peak is at 522nm and coated with SiO 2 The post peak was red shifted because this comparative example was prepared to quantum dots first and then coated, rather than synthesized in situ.
Characterization and Performance testing
Fig. 1 is an SEM image of the lead organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1. As shown in fig. 1, the lead organic complex in the large size and the perovskite particles in the small size are well combined together. SEM images of all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder prepared in examples 2-12 are similar to those of FIG. 1.
Fig. 2 is an XRD pattern of the lead organic complex prepared in example 1. As can be seen from fig. 2, step S1 of example 1 successfully prepares a lead organic complex. The XRD pattern of the lead organic complex prepared in step S1 of examples 2 to 12 is similar to that of fig. 2.
Fig. 3 is an XRD chart of the lead-organic complex coated all-inorganic lead-halogen perovskite nano-crystalline phosphor prepared in example 1. As can be seen from FIG. 3, the all-inorganic lead-halogen perovskite nanocrystalline phosphor coated by the lead-organic complex is successfully prepared in example 1. XRD of all inorganic lead-halogen perovskite nano-crystal fluorescent powder described in examples 2-12 is similar to that of figure 3.
Fig. 4 is a photoluminescence chart of the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1. As shown in FIG. 4, the fluorescent peak position of the all-inorganic lead-halogen perovskite nano-crystalline phosphor prepared in example 1 is 519nm, and the half-peak width is 17nm. Photoluminescence patterns of all-inorganic lead-halogen perovskite nanocrystalline phosphors described in examples 2-12 are similar to those of fig. 4.
FIG. 5 is a graph showing the change of fluorescence intensity of the lead-organic complex-coated all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1 with the time of soaking in water. As can be seen from fig. 5, the all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1 is soaked in water for more than 400h, and still maintains more than 65% of the initial fluorescence intensity, which indicates that the all-inorganic lead-halogen perovskite nanocrystalline phosphor prepared in example 1 has excellent stability. The graph of the change of the fluorescence intensity of the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder prepared in the embodiments 2 to 12 along with the water soaking time is similar to that in fig. 5, which shows that the all-inorganic lead-halogen perovskite nanocrystalline fluorescent powder prepared in the embodiments 2 to 12 has better stability.
Fig. 6 is an electroluminescence diagram of LED devices prepared from the lead-organic complex-coated all-inorganic lead-halogen perovskite nanocrystalline phosphor and blue light chips and commercial red powder prepared in example 1. As shown in fig. 6, the chip with blue light emission in the electro-photoluminescence spectrogram, the all-inorganic lead-halogen perovskite nano-crystal fluorescent powder coated by the lead organic complex with green light color emission and the commercial red powder with red light emission are formed.
Fig. 7 is a graph of the fluorescence quantum yield of the lead-organic complex coated all-inorganic lead-halogen perovskite nano-crystalline phosphor prepared in example 1, and it can be seen from fig. 7 that the quantum yield of the prepared lead-organic complex coated all-inorganic lead-halogen perovskite nano-crystalline phosphor reaches 48.5%. The fluorescence quantum yield of the lead organic complex coated all-inorganic lead halogen perovskite nano crystal fluorescent powder prepared in the examples 2 to 12 is basically consistent with that of the example 1.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. A preparation method of lead organic complex coated all-inorganic lead halogen perovskite nanocrystalline fluorescent powder is characterized by comprising the following steps:
s1, adding metal halide PbX 2 Adding mandelic acid and oleylamine into the octadecene solution, and stirring for 0.5 to 5 hours at the temperature of 60 to 160 ℃ to obtain a solution of a Pb-mandelic acid organic complex;
s2, adding an oleic acid solution of cesium carbonate into a solution of a Pb-mandelic acid organic complex, reacting for 3S to 30min at the temperature of 80 to 180 ℃ in an inert atmosphere, and performing post-treatment to obtain the inorganic lead-halogen perovskite nanocrystalline fluorescent powder coated by the lead organic complex;
the metal halide PbX 2 Selected from PbCl 2 、PbBr 2 、PbI 2 One or more of; the mandelic acid is selected from one of DL-mandelic acid, D-mandelic acid and L-mandelic acid;
the metal halide PbX 2 The mol ratio of the mandelic acid to the mandelic acid is 1 (0.5 to 5);
cesium ions and metal halide PbX in the oleic acid solution of cesium carbonate 2 The molar ratio of (0.5 to 2) to (1).
2. The method for preparing the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor according to claim 1, wherein the metal halide PbX 2 The molar ratio of the mandelic acid to the mandelic acid is 1 (0.8-2).
3. The method for preparing the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor according to claim 2, wherein the metal halide PbX 2 The molar ratio to mandelic acid was 1:1.
4. The method for preparing lead organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor according to claim 1, wherein cesium ions in an oleic acid solution of cesium carbonate and a metal halide PbX 2 The molar ratio of (0.8 to 1.2) to (1).
5. The preparation method of the lead organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor according to claim 1, wherein the stirring temperature is 120 to 160 ℃ and the stirring time is 0.5 to 2h.
6. The preparation method of the lead organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor according to claim 1, wherein the reaction temperature is 140 to 160 ℃ and the reaction time is 3 to 60s.
7. An all-inorganic lead-halogen perovskite nanocrystalline phosphor coated with a lead organic complex, characterized by being prepared by the preparation method of any one of claims 1~6.
8. The use of the lead-organic complex coated all-inorganic lead-halogen perovskite nanocrystalline phosphor of claim 7 in the display field.
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