CN111073635A - Multilevel chiral luminescence reinforced composite material and preparation method thereof - Google Patents

Multilevel chiral luminescence reinforced composite material and preparation method thereof Download PDF

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CN111073635A
CN111073635A CN201911270495.9A CN201911270495A CN111073635A CN 111073635 A CN111073635 A CN 111073635A CN 201911270495 A CN201911270495 A CN 201911270495A CN 111073635 A CN111073635 A CN 111073635A
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王宇
李震
颜岩
赵佳奇
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Jilin University
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Abstract

A multilevel chiral luminescence reinforced composite material of silver nanorod composite silicon dioxide and cysteine coated with all-inorganic perovskite quantum dots and a preparation method thereof belong to the technical field of chiral luminescent material preparation. The method comprises the steps of obtaining a one-dimensional silver nanorod through polyol reaction, and obtaining AgNR @ SiO through hydrolysis of TEOS and APTES2And then stirring with cysteine solution at room temperature to obtain AgNR @ SiO2The @ L-cys complex, which is finally injected with heatCompounding the prepared all-inorganic perovskite Quantum Dots (QDs) to prepare AgNR @ SiO with a multistage nano structure2@ L-cys @ QDs chiral luminescence enhanced composite material. The material has a rod-like shape, and perovskite quantum dots are uniformly distributed on the surface, wherein AgNR @ SiO2@L‑cys@CsPbBr3Has 87 times luminous enhancement. The invention has the advantages of low preparation cost, large-scale preparation, simple method, easy operation, good repeatability and the like.

Description

Multilevel chiral luminescence reinforced composite material and preparation method thereof
Technical Field
The invention belongs to the technical field of preparation of chiral luminescent materials, and particularly relates to a multilevel chiral luminescence enhanced composite material (AgNR @ SiO) with perovskite quantum dots coated with silver nanorod composite silicon dioxide and cysteine2@ L-cys @ QDs) and a preparation method thereof.
Background
Chirality is an essential attribute possessed by asymmetric center, symmetric plane and anti-axial structure, and it exists widely in nature. This property has not only a wide range of applications in the fields of nonlinear optics, spintronics, etc., but also is closely related to biological and pharmaceutical sciences. In the past decades, chiral inorganic nanomaterials have attracted considerable attention due to their excellent optical and chemical properties, compared to chiral organic molecules, and have shown great potential in the fields of displays, lighting, etc. Among them, chiral perovskites have been widely studied by researchers due to their unique physical and chemical properties.
For example, the Tang project group at the university of science and technology in Huazhong successfully synthesized chiral (R-and S- α -PEA) PbI3Perovskites and have application in the detection of circularly polarised light (Nat commun.2019,10,1927) because they can combine chiral organic-induced circularly polarised light sensitive absorption with efficient charge transport by inorganic scaffolds. The Xu subject group at southern university has prepared chiral lead-perovskite halide nanowires for the study of second-order nonlinear optics, which exhibit high efficiency of Second Harmonic Generation (SHG), high polarizability and chiral nonlinear optical effects. (Nano Lett.2018,18, 5411-5417).
The research results fully show the attractive prospect of the chiral perovskite material. However, nano perovskite materials generally have low quantum efficiency and are not prone to generate chiral structures without the participation of chiral amines. Therefore, the perovskite nano particles and the noble metal nano rods are combined, so that the luminous efficiency can be enhanced, and the luminescent material with the multilevel chiral structure can be prepared by utilizing the chiral arrangement of the nano rods.
Disclosure of Invention
The invention aims to provide a multilevel chiral luminescence enhanced composite material (AgNR @ SiO) with perovskite quantum dots coating silver nanorod composite silicon dioxide and cysteine2@ L-cys @ QDs) and a preparation method thereof. AgNR stands for silver nanorod, SiO2Is silicon dioxide, L-cys stands for L-cysteine, and QDs stands for perovskite quantum dots.
The method takes silver nitrate, ethylene glycol, Tetraethoxysilane (TEOS), 3-Aminopropyltriethoxysilane (APTES), ammonia water, L-cysteine, octadecene, oleic acid, oleylamine, lead halide, manganese bromide, zinc bromide, cesium carbonate and the like as raw materials, obtains a one-dimensional silver nanorod through polyol reduction reaction, and then obtains AgNR @ SiO through hydrolysis of TEOS and APTES2And then stirring with cysteine solution at room temperature to obtain AgNR @ SiO2The @ L-cys compound is finally compounded with perovskite Quantum Dots (QDs) prepared by a thermal injection method to prepare AgNR @ SiO with a multistage nano structure2@ L-cys @ QDs chiral luminescence enhanced composite material. The diameter of the silver nanorod is 75-85 nanometers, the length of the silver nanorod is 8-11 micrometers, the thickness of the coated silicon dioxide layer and the thickness of the coated cysteine layer are 1.5-3 nanometers, the synthesized composite material has a rod-shaped appearance, and perovskite quantum dots are uniformly distributed on the surface.
The invention relates to a multilevel chiral luminescence enhanced composite material (AgNR @ SiO)2@ L-cys @ QDs), which comprises the following steps:
a) adding polyvinylpyrrolidone (PVP), silver nitrate and ferric trichloride into ethylene glycol, dissolving, putting into an oil bath, heating, centrifugally washing to obtain silver nanorods (AgNR), and dispersing in deionized water to obtain a silver nanorod (AgNR) solution;
b) dispersing the silver nanorod (AgNR) solution obtained in the step a) in isopropanol, then adding TEOS and APTES into the solution, stirring uniformly, and then adding ammoniaWater solution, centrifugally washing the reaction crude product, and dispersing in deionized water to obtain silver nanorods (AgNR @ SiO) coated with silicon dioxide2) A solution;
c) the silver nano rod (AgNR @ SiO) coated by the silicon dioxide obtained in the step b)2) Mixing the solution and deionized water, adding cysteine solution, mixing, stirring, centrifuging, and drying to obtain composite material (AgNR @ SiO) of cysteine and silicon dioxide coated silver nanorod2@L-cys)；
d) Adding cesium carbonate and oleic acid into octadecene, and heating and reacting under the atmosphere of nitrogen to obtain a cesium oleate precursor;
e) adding metal halide (lead halide, manganese bromide or zinc bromide) into octadecene, then adding oleic acid and oleylamine, fully stirring at high temperature and under a nitrogen atmosphere, adding the cesium oleate precursor prepared in the step d) after dissolving, immediately putting the cesium oleate precursor into an ice-water bath for cooling after reaction, centrifugally washing a crude product, and dispersing the crude product in n-hexane to obtain perovskite Quantum Dots (QDs);
f) coating the cysteine and silicon dioxide obtained in the step c) on the silver nano rod composite material (AgNR @ SiO)2Mixing and stirring the normal hexane solution of @ L-cys) and the perovskite Quantum Dots (QDs) obtained in the step e) to obtain the multistage chiral luminescence enhanced composite material (AgNR @ SiO)2@L-cys@QDs)。
Step a) adding 0.15-0.30 g of PVP into 20-30 mL of ethylene glycol, stirring for dissolving, adding 0.2-0.4 g of silver nitrate, stirring for dissolving, adding 2.5-5.0 g (with the concentration of 400-800 mmol/L) of ethylene glycol solution of ferric trichloride, stirring uniformly, transferring into an oil bath pot, and stirring for 4-8 hours at the temperature of 120-140 ℃; centrifugally washing the crude product, and dispersing the washed crude product in 10-20 ml of deionized water to obtain a silver nanorod (AgNR) water solution;
step b) adding 2-4 mL of silver nanorod aqueous solution into 10-30 mL of isopropanol, then adding 5-20 microliters of TEOS and 5-10 microliters of APTES, uniformly stirring, adding 1-2 mL of ammonia aqueous solution, and stirring and reacting at room temperature for 2-4 hours; centrifugally washing the crude product, and dispersing the washed crude product in 10-20 mL of deionized water to obtain a silver nanorod (AgNR @ SiO) coated with silicon dioxide2) An aqueous solution;
step c) is to mix 10-20 mL of AgNR @ SiO2Adding the aqueous solution into 15-25 mL of deionized water, then adding 5-15 mL of 1-5 mM L-cys aqueous solution, and stirring at room temperature for 6-24 hours; centrifugally washing and drying the crude product to obtain the solid composite material (AgNR @ SiO) of the cysteine and silicon dioxide coated silver nanorod2@L-cys)；
Step d) adding 0.4-1 g of cesium carbonate and 1-3 mL of oleic acid into 20-40 mL of octadecene, stirring for 10-30 minutes at 100-120 ℃ in a nitrogen atmosphere, and then heating to 140-160 ℃ to completely react the oleic acid and the cesium carbonate to obtain a cesium oleate precursor;
step e) adding 0.1-0.4 g of metal halide (one or two of lead halide, manganese bromide and zinc bromide) into 10-30 mL of octadecene, stirring for 0.2-1 hour at 100-120 ℃ under a nitrogen atmosphere, then adding 1-3 mL of oleylamine and 1-3 mL of oleic acid, and heating to 140-160 ℃ until the solid is completely dissolved. Then, quickly adding 1-2 mL of cesium oleate precursor into the solution, reacting for 5-10 s, immediately putting into ice water for cooling, centrifugally washing a crude product, and dispersing in 20-40 mL of n-hexane to obtain a perovskite Quantum Dot (QDs) solution;
step f) is to coat the cysteine and the silicon dioxide on the solid composite material (AgNR @ SiO) of the silver nano rod2@ L-cys) is added into 20-40 mL of normal hexane, 5-10 mL of perovskite Quantum Dot (QDs) solution is added, and stirring is carried out for 6-24 h to obtain the multistage chiral luminescence enhanced composite material (AgNR @ SiO)2@L-cys@QDs)。
The invention provides a multilevel chiral luminescence enhanced composite material (AgNR @ SiO)2@ L-cys @ QDs), has the characteristics of low preparation cost, simple method, easy operation, reliable production process, good repeatability, large yield and the like. The composite material has obvious chiral signals and good luminescence property.
Drawings
FIG. 1: scanning electron micrographs of silver nanorods (AgNRs) prepared in example 1; it can be seen that the silver nanorods have a uniform morphology and a smooth surface, a length of about 10 micrometers, and a diameter of about 80 nanometers;
FIG. 2: an X-ray diffraction (XRD) spectrum of the silver nanorods (AgNRs) prepared in example 1; it can be seen that all diffraction peaks of the sample corresponded to the standard card of silver (JCPDS NO.04-0783) and that there was no impure phase.
FIG. 3: example 1A preparation of a hierarchical nanostructured AgNR @ SiO2Scanning electron microscope photographs of the composite material; the surface of the nano rod is smooth, which shows that the silicon dioxide can be uniformly coated on the silver nano rod.
FIG. 4: AgNR @ SiO prepared in example 12The graph shows that 200-320nm shows an interband absorption enhanced optical activity signal of cysteine (cys) molecular arrangement, and 350-450nm shows a chiral signal of silver nanorod arrangement, which indicates that AgNR @ SiO is2Successfully compounded with L-cys to form a multilevel chiral composite material AgNR @ SiO2@L-cys。
FIG. 5: example 1 preparation of perovskite Quantum dots CsPbBr3The high-resolution transmission electron microscope picture of the QDs shows that the QDs have good crystallinity, and the size of the QDs is about 15-25 nm;
FIG. 6: example 1 preparation of all-inorganic perovskite CsPbBr3The X-ray diffraction (XRD) spectrum of the QDs material, all diffraction peaks of the sample correspond to a standard card (JCPDS No.54-0752) of a cubic phase thereof;
FIG. 7: example 1A preparation of a hierarchical nanostructured AgNR @ SiO2@L-cys@CsPbBr3Transmission electron microscope pictures of the composite material; it can be seen that CsPbBr is uniformly distributed on the surface of the silver nanorod coated with silicon dioxide and cysteine molecules3QDs；
FIG. 8: AgNR @ SiO prepared in example 12@L-cys@CsPbBr3X-ray diffraction pattern of the material, all peaks with AgNRs and CsPbBr3Standard spectra correspond (strong peaks correspond to silver nanorods; marked peaks correspond to cubic phase CsPbBr)3QDs)。
FIG. 9: AgNR @ SiO prepared in example 12@L-cys@CsPbBr3MaterialThe chiral signals of about 200-320nm, 350-450nm and 500nm respectively correspond to the signals of cysteine molecular arrangement, the signals of silver nanorod arrangement and CsPbBr3The signal caused by exciton absorption proves AgNRs and SiO2L-cys with CsPbBr3QDs successfully complex.
FIG. 10: example 1 fluorescence emission spectra of prepared samples; this sample is compared to pure CsPbBr3QDs has the effect of luminescence enhancement, AgNR @ SiO in example 12@L-cys@CsPbBr3For pure CsPbBr3Has 87 times enhancement of the luminous intensity.
FIG. 11: CsPbCl prepared in examples 5 to 83、CsPbClxBr3-x、CsPbBrxI3-x、CsPbI3Fluorescence emission spectrum of the sample; it can be seen from the above that the emission wavelength of the sample can be adjusted by changing the kind and content of the anions, and the emission wavelengths of the curves 1-4 are 402 nm, 456 nm, 599 nm and 689nm respectively.
FIG. 12: CsMn prepared in example 9 and example 10xPb1-xBr3、CsZnxPb1-xBr3Fluorescence emission spectrum of the sample. The emission wavelengths of curve 1 and curve 2 are 510, 512nm, respectively.
Detailed Description
Example 1
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsPbBr3) The preparation process comprises the following concrete five steps:
1. synthesis of aqueous solution of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
adding 2mL of the silver nanorod aqueous solution prepared in the step 1 into 20mL of isopropanol, then adding 20 microliters of TEOS and 10 microliters of APTES, stirring uniformly, and adding 1.9mL of ammonia aqueous solution. The solution was stirred at room temperature for 2 h. The crude product was then washed centrifugally and finally dispersed in 10mL deionized water to give AgNR @ SiO2An aqueous solution.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4.CsPbBr3Synthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so as to obtain a cesium oleate precursor solution.
0.276 g of lead bromide was added to 20mL of octadecene, stirred at 120 ℃ for 0.5 hour under a nitrogen atmosphere, followed by addition of 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the lead bromide was completely dissolved. And then, quickly adding 1.6mL of cesium oleate precursor solution into the solution, reacting for 5s, immediately putting the solution into ice water for cooling, centrifugally washing the crude product, and dispersing the crude product into 40mL of n-hexane to obtain CsPbBr3Perovskite quantum dot solution.
5. Multistage chiral nano luminescent reinforced composite AgNR @ SiO2@L-cys@CsPbBr3The synthesis of (2):
mixing 40mL of the solution obtained in the step 3 with 5mL of the solution obtained in the step 4 at room temperature, and stirring for 24 hours to obtain the AgNR @ SiO of the invention2@L-cys@CsPbBr3And (3) enhancing the composite luminescent material.
A scanning electron microscope photo of the AgNRs with the silver nanorod structure is shown in figure 1, and the AgNRs with the silver nanorod structure can be shown to have a uniform appearance and a smooth surface, wherein the length of the AgNRs is about 8-11 micrometers, and the diameter of the AgNRs is about 75-85 nanometers. X-ray diffraction of AgNRsThe (XRD) spectrum (FIG. 2) shows that all diffraction peaks of the sample can correspond to the standard card for silver (JCPDS 04-0783). AgNR @ SiO2The scanning electron micrograph of the composite material is shown in fig. 3, and the sample has a smooth surface, which indicates that the silver nanorods are uniformly coated with the silicon dioxide. AgNR @ SiO2The Circular Dichroism (CD) of the @ L-Cys composite material is shown in figure 4, the CD signal of 200-320nm is the intercand absorption enhanced optical activity of the molecular arrangement of cysteine (Cys), and the CD signal of 350-450nm is the chiral signal of the silver nanorod arrangement. FIG. 5 shows the preparation of an all-inorganic perovskite CsPbBr3The high resolution transmission electron microscope pictures of QDs show good crystallinity with a size of about 15-25 nm. CsPbBr3The X-ray diffraction (XRD) pattern of the QDs material (fig. 6) shows that all diffraction peaks of the sample can be mapped to the standard card of its cubic phase (JCPDS 54-0752). AgNR @ SiO with multi-stage nano structure2@L-cys@CsPbBr3It can be seen that CsPbBr is uniformly distributed on the surface of the silver nanorod coated with silicon dioxide and cysteine molecules3QDs, whose X-ray diffraction pattern is shown in FIG. 8, all peaks were observed with silver (JCPDS04-0783) and CsPbBr3(JCPDS 54-0752) standard spectra. The circular dichroism chromatogram of the material is shown in figure 9, and chiral signals at about 200-320nm, 350-450nm and 500-550 nm respectively correspond to a signal of cysteine molecular arrangement, a signal of silver nanorod arrangement and CsPbBr3The exciton absorbs the induced signal. AgNR @ SiO2@L-cys@CsPbBr3The fluorescence emission spectrum of the sample is shown in FIG. 10, relative to pure CsPbBr3Has 87 times enhancement of the luminous intensity.
Example 2
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsPbCl3) The preparation process comprises the following concrete five steps:
1. synthesis of aqueous solution of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4.CsPbCl3Synthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. Then 0.209 g of lead chloride was added to 20mL of octadecene, stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the lead chloride was completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. AgNR @ SiO with multi-stage chiral nano luminescent structure2@L-cys@CsPbCl3Synthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsPbCl3And (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsPbCl3Compared with perovskite quantum dots, the perovskite quantum dots have the advantages of 38 timesThe luminescence is enhanced.
Example 3
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsPbClxBr3-x) The preparation process comprises the following concrete five steps:
1. synthesis of aqueous solution of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4.CsPbClxBr3-xSynthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. Then 0.1112 g of lead chloride and 0.1468 g of lead bromide were added to 20mL of octadecene and stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the solids were completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. AgNR @ SiO with multi-stage chiral nano luminescent structure2@L-cys@CsPbClxBr3-xSynthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsPbClxBr3-xAnd (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsPbClxBr3-xThe perovskite quantum dots have 23 times luminous enhancement compared with the perovskite quantum dots.
Example 4
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsPbBrxI3-x) The preparation process comprises the following concrete five steps:
1. synthesis of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. Centrifugal washing of the crude productThereafter, the solid product was dried at 60 ℃ and dispersed in 40mL of an n-hexane solution.
4.CsPbBrxI3-xSynthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. 0.1468 g of lead bromide and 0.1844 g of lead iodide were then added to 20mL of octadecene and stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the solids were completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. AgNR @ SiO with multi-stage chiral nano luminescent structure2@L-cys@CsPbBrxI3-xSynthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsPbBrxI3-xAnd (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsPbBrxI3-xThe perovskite quantum dots have 10 times luminous enhancement compared with the perovskite quantum dots.
Example 5
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsPbI3) The preparation process comprises the following concrete five steps:
1. synthesis of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4.CsPbI3Synthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. 0.3467 g of lead iodide were then added to 20mL of octadecene and stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the solid was completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. AgNR @ SiO with multi-stage chiral nano luminescent structure2@L-cys@CsPbI3Synthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsPbI3And (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsPbI3The perovskite quantum dots have 4 times luminous enhancement compared with the perovskite quantum dots.
Example 6
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsMnxPb1-xBr3) The preparation process comprises the following concrete five steps:
1. synthesis of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4.CsMnxPb1-xSynthesizing Br perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. Then 0.276 g of lead bromide and 0.1 g of manganese bromide were added to 20mL of octadecene, stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the solids were completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. Has multilevel chiral nano hairOptical structure AgNR @ SiO2@L-cys@CsMnxPb1-xBr3Synthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsMnxPb1-xBr3And (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsMnxPb1-xBr3The perovskite quantum dots have 3 times luminous enhancement compared with the perovskite quantum dots.
Example 7
Composite material (AgNR @ SiO) with multistage chiral luminescence enhancement2@L-cys@CsZnxPb1-xBr3) The preparation process comprises the following concrete five steps:
1. synthesis of silver nanorods (AgNRs):
0.2 g of PVP is added into 25mL of ethylene glycol, 0.25 g of silver nitrate is added after stirring and dissolving, 3.75 g (with the concentration of 600 mmol/L) of ethylene glycol solution of ferric trichloride is added after dissolving, the mixture is transferred into an oil bath kettle after even stirring, and the mixture is stirred for 5 hours at the temperature of 130 ℃. The crude product was then washed by centrifugation and finally dispersed in 10ml of deionized water.
2. AgNR @ SiO with multi-stage nano structure2Synthesis of the composite material:
2mL of the aqueous silver nanorod solution prepared in step 1 was added to 20mL of isopropanol, followed by 20. mu.L of TEOS and 10. mu.L of APTES, followed by 1.9mL of aqueous ammonia solution. The solution was stirred at room temperature for 2 h. The crude product was then washed by centrifugation and finally dispersed in 10mL of deionized water.
3. AgNR @ SiO with multi-stage nano structure2Synthesis of @ L-cys composite:
10mL of AgNR @ SiO obtained in step 22The aqueous solution was added to 25mL of deionized water, followed by addition of 12.5mL of an aqueous solution of Cys (concentration: 1mM), and the mixture was stirred at room temperature for 24 hours. After the crude product was washed by centrifugation, it was dried at 60 ℃ to give a solid product, which was dispersed in 40mL of n-hexane solution.
4. All-inorganic CsZnxPb1-xBr3Synthesis of perovskite quantum dots:
0.814 g of cesium carbonate and 2.5mL of oleic acid were added to 30mL of octadecene, stirred at 120 ℃ for 20 minutes under a nitrogen atmosphere, and then heated to 160 ℃ to completely react the oleic acid with the cesium carbonate, so that a cesium oleate precursor solution was obtained. Then 0.276 g of lead bromide and 0.1 g of zinc bromide were added to 20mL of octadecene, stirred at 120 ℃ for 0.5 hour under nitrogen, followed by 2mL of oleylamine and 2mL of oleic acid, and warmed to 160 ℃ until the solids were completely dissolved. Then, 1.6mL of cesium oleate precursor is rapidly added into the solution, the solution is immediately placed into ice water for cooling after reacting for 5s, and the crude product is dispersed in 40mL of n-hexane after centrifugal washing.
5. AgNR @ SiO with multi-stage chiral nano luminescent structure2@L-cys@CsZnxPb1-xBr3Synthesis of the reinforced composite material:
mixing and stirring the product obtained in the step 3 (40mL) and the product obtained in the step 4 (5 mL) at room temperature for 24 hours to obtain AgNR @ SiO2@L-cys@CsZnxPb1-xBr3And (3) enhancing the composite luminescent material.
The product obtained in this example has similar structural characteristics to those of example 1, and is pure CsZnxPb1-xBr3The perovskite quantum dots have 19 times luminous enhancement compared with the perovskite quantum dots.

Claims (9)

1. A preparation method of a multilevel chiral luminescence reinforced composite material comprises the following steps:
a) adding polyvinylpyrrolidone, silver nitrate and ferric trichloride into ethylene glycol, dissolving, putting into an oil bath, heating, centrifugally washing to obtain silver nanorods, and dispersing in deionized water to obtain a silver nanorod aqueous solution;
b) dispersing the silver nanorod solution obtained in the step a) in isopropanol, then adding ethyl orthosilicate and 3-aminopropyltriethoxysilane into the solution, stirring uniformly, then adding an ammonia water solution, centrifugally washing a reaction crude product, and dispersing in deionized water to obtain a silicon dioxide coated silver nanorod solution;
c) mixing the silver nanorod solution coated with silicon dioxide obtained in the step b) with deionized water, adding a cysteine solution into the mixture, mixing and stirring the mixture, and centrifugally drying the mixture to obtain a composite material of cysteine and the silver nanorods coated with silicon dioxide;
d) adding cesium carbonate and oleic acid into octadecene, and heating and reacting under the atmosphere of nitrogen to obtain a cesium oleate precursor;
e) adding lead halide, manganese bromide or zinc bromide into octadecene, then adding oleic acid and oleylamine, fully stirring at high temperature and under a nitrogen atmosphere, adding the cesium oleate precursor prepared in the step d) after dissolving, immediately putting the cesium oleate precursor into an ice-water bath for cooling after reaction, and dispersing the crude product in n-hexane after centrifugal washing to obtain perovskite quantum dots;
f) mixing and stirring the n-hexane solution of the cysteine and silicon dioxide coated silver nanorod composite material obtained in the step c) and the perovskite quantum dots obtained in the step e) to obtain the multistage chiral luminescence enhanced composite material AgNR @ SiO2@ L-cys @ QDs, AgNR stands for silver nanorod, SiO2For silicon dioxide, L-cys stands for cysteine, and QDs stands for perovskite quantum dots.
2. The method of claim 1, wherein the method comprises the following steps: step a) adding 0.15-0.30 g of polyvinylpyrrolidone into 20-30 mL of ethylene glycol, stirring for dissolving, adding 0.2-0.4 g of silver nitrate, stirring for dissolving, adding 2.5-5.0 g (with the concentration of 400-800 mmol/L) of ethylene glycol solution of ferric trichloride, stirring uniformly, transferring into an oil bath pot, and stirring for 4-8 hours at the temperature of 120-140 ℃; and centrifugally washing the crude product, and dispersing the washed crude product in 10-20 ml of deionized water to obtain a silver nanorod water solution.
3. The method of claim 1, wherein the method comprises the following steps: step b) adding 2-4 mL of silver nanorod aqueous solution into 10-30 mL of isopropanol, then adding 5-20 microliters of ethyl orthosilicate and 5-10 microliters of 3-aminopropyltriethoxysilane, uniformly stirring, adding 1-2 mL of ammonia water solution, and stirring and reacting at room temperature for 2-4 hours; and dispersing the crude product after centrifugal washing in 10-20 mL of deionized water to obtain a silver nanorod water solution coated with silicon dioxide.
4. The method of claim 1, wherein the method comprises the following steps: step c) adding 10-20 mL of silicon dioxide coated silver nanorod solution into 15-25 mL of deionized water, then adding 5-15 mL of 1-5 mM cysteine aqueous solution, and stirring at room temperature for 6-24 hours; and centrifugally washing and drying the crude product to obtain the solid composite material of the cysteine and the silicon dioxide coated silver nanorods.
5. The method of claim 1, wherein the method comprises the following steps: and d) adding 0.4-1 g of cesium carbonate and 1-3 mL of oleic acid into 20-40 mL of octadecene, stirring for 10-30 minutes at 100-120 ℃ in a nitrogen atmosphere, and then heating to 140-160 ℃ to completely react the oleic acid and the cesium carbonate to obtain an oleic acid cesium precursor.
6. The method of claim 1, wherein the method comprises the following steps: step e) adding 0.1-0.4 g of metal halide into 10-30 mL of octadecene, stirring for 0.2-1 hour at 100-120 ℃ under a nitrogen atmosphere, then adding 1-3 mL of oleylamine and 1-3 mL of oleic acid, and heating to 140-160 ℃ until the solid is completely dissolved; and then, quickly adding 1-2 mL of cesium oleate precursor into the solution, reacting for 5-10 s, immediately putting into ice water for cooling, centrifugally washing the crude product, and dispersing in 20-40 mL of n-hexane to obtain a perovskite quantum dot solution.
7. The method of claim 6, wherein the method comprises the following steps: the metal halide is one or two of lead halide, manganese bromide and zinc bromide.
8. As claimed in claim1, the preparation method of the multilevel chiral luminescence reinforced composite material is characterized in that: step f) adding the solid composite material of the cysteine and the silicon dioxide coated silver nanorod into 20-40 mL of n-hexane, adding 5-10 mL of perovskite quantum dot solution, and stirring for 6-24 h to obtain the multistage chiral luminescence enhanced composite material AgNR @ SiO2@L-cys@QDs。
9. A preparation method of a multilevel chiral luminescence reinforced composite material is characterized by comprising the following steps: is prepared by the method of any one of claims 1 to 8.
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