CN117487548B - Perovskite quantum dot composite material, preparation method and application - Google Patents
Perovskite quantum dot composite material, preparation method and application Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 54
- 239000002096 quantum dot Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000003960 organic solvent Substances 0.000 claims abstract description 40
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002808 molecular sieve Substances 0.000 claims abstract description 17
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000011148 porous material Substances 0.000 claims abstract description 4
- 238000004020 luminiscence type Methods 0.000 claims description 36
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 18
- 238000001514 detection method Methods 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 9
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000002189 fluorescence spectrum Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 230000003287 optical effect Effects 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 4
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 24
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 15
- 239000000203 mixture Substances 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 12
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 8
- 235000019441 ethanol Nutrition 0.000 description 7
- 239000002904 solvent Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 238000005119 centrifugation Methods 0.000 description 5
- 230000005284 excitation Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000001748 luminescence spectrum Methods 0.000 description 4
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002161 passivation Methods 0.000 description 2
- 238000005424 photoluminescence Methods 0.000 description 2
- 238000000103 photoluminescence spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000003495 polar organic solvent Substances 0.000 description 1
- 239000005373 porous glass Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000000844 transformation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
The invention discloses a perovskite quantum dot composite material, a preparation method and application thereof, and belongs to the field of optical sensing. The perovskite quantum dot composite material is CsPbBr 3/Cs4PbBr6 @MCM-41 composite material; csPbBr 3/Cs4PbBr6 is loaded in the pore canal of MCM-41 molecular sieve. The CsPbBr 3/Cs4PbBr6 @MCM-41 composite material has the advantages of high response sensitivity, good reversibility, good repeatability, high response speed and strong controllability of an organic solvent, and can be used for detecting the polarity of the organic solvent.
Description
Technical Field
The invention belongs to the technical field of optical sensing, and particularly relates to a perovskite quantum dot composite material, a preparation method and application thereof.
Background
Inorganic perovskite materials have shown wide application in photovoltaic and photovoltaic devices due to their solution processability, tunable band gap, ultra-high luminescent quantum efficiency and excellent photovoltaic properties. In recent years, perovskite materials are susceptible to reversible chemical and structural transformations under the stimulus of light, heat, pressure, water and chemical environments due to ease of preparation and ease of variation and degradation, and lead halide perovskite among them is an attractive stimulus-responsive luminescent material due to its low energy of formation and excellent optical properties.
However, lead halide perovskite is unstable, and the synthesis of lead halide perovskite in porous materials is originally a method for improving perovskite stability, and materials reported at present are zeolite, porous SiO 2, porous Al 2O3, porous glass and the like. The CsPbBr 3 @mesoporous SiO 2、EMT-CsPbBr3 and other composite materials are used in the fields of optical sensing and the like.
At present, the fluorescent materials suitable for detecting the polarity of the organic solvent are extremely small in quantity, poor in stability, small in application range and poor in controllability. Gan et al disperse CsPbBr 3 in polar organic solvent, judge the polarity size according to its fluorescence quenching degree, such detection mode not only has a smaller detection range, poor stability, and poor fitting property with the fitting curve, and poor repeatability.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a perovskite quantum dot composite material, a preparation method and application thereof, and the CsPbBr 3@Cs4PbBr6/MCM-41 composite material obtained by compounding CsPbBr 3、Cs4PbBr6 and an MCM-41 molecular sieve can be used for detecting the polarity of an organic solvent, and has the advantages of good detection stability and wide application range.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
The perovskite quantum dot composite material is CsPbBr 3/Cs4PbBr6 @MCM-41 composite material, and CsPbBr 3/Cs4PbBr6 is loaded in a pore canal of an MCM-41 molecular sieve.
The perovskite quantum dot composite material is applied to polarity detection of an organic solvent.
The method for detecting the polarity of the organic solvent by using the perovskite quantum dot composite material comprises the following steps:
Dispersing the perovskite quantum dot composite material in an organic solvent to be detected, and carrying out peak-splitting fitting on a fluorescence spectrum under 365nm ultraviolet excitation to obtain fluorescence intensities of a blue light luminescence peak and a green light luminescence peak; the relative intensity values of the blue light luminescence peak and the green light luminescence peak are brought into a polar detection model curve, and the polarity of the organic solvent is calculated;
The relative intensities of the blue light emission peak and the green light emission peak are as follows: blue light emission peak intensity/green light emission peak intensity=i B/IG; the central wavelength of the blue light emission peak is 460-490nm, and the central wavelength of the green light emission peak is 500-530nm.
And performing Gaussian peak-splitting fitting on a fluorescence spectrum excited by 365nm ultraviolet light by adopting Origin to obtain a blue light luminescence peak with a wavelength center of 460-490nm and a green light luminescence peak with a wavelength center of 500-530 nm.
As a preferred embodiment of the invention, the relative intensity values of blue light luminescence peaks and green light luminescence peaks of the perovskite quantum dot composite material in different organic solvents are subjected to numerical fitting with the polarity of the organic solvents, and the equation for obtaining a polarity detection model curve is as follows: Wherein a 1、A2、X0、dx is a fixed value, a 1＝1.71075,A2＝0.17707,X0＝4.48781,dx =0.17301, f is a relative intensity value of a blue light emission peak and a green light emission peak, and P is a polarity of the organic solvent.
More preferably, the method for detecting the polarity of the solvent by using the perovskite quantum dot composite material comprises the following steps:
(1) Dispersing 0.03g of the perovskite quantum dot composite material in an organic solvent to be detected, measuring a fluorescence luminescence spectrum under 365nm ultraviolet excitation, and carrying out Gaussian peak-splitting fitting on the fluorescence luminescence spectrum by adopting Origin to obtain a blue light luminescence peak with a wavelength center of 460-490nm and a green light luminescence peak with a wavelength center of 500-530 nm; substituting the fluorescence intensity ratio of the blue light luminescence peak and the green light luminescence peak into a polar detection model curve, and calculating to obtain the polarity of the organic solvent to be detected; the organic solvent to be detected is an organic solvent with unknown polarity;
(2) Drawing a polar detection model curve: dispersing the perovskite quantum dot composite material in dichloromethane, 1-butanol, absolute ethyl alcohol, ethyl acetate, 1, 4-dioxane and acetone organic solvents according to the method of the step (1), testing fluorescence luminescence spectrum under 365nm light excitation, obtaining relative intensity values of blue light luminescence peak and green light luminescence peak by peak separation, and drawing standard curves of polarities of different organic solvents and the relative intensity values of the blue light luminescence peak and the green light luminescence peak of corresponding materials to obtain a polarity detection model curve.
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) Mixing a DMF solution of PbBr 2 with a molecular sieve MCM-41, sequentially carrying out ultrasonic treatment, drying and calcining to obtain PbBr 2 @MCM-41;
(2) Adding PbBr 2 @MCM-41 into a CsBr hydroalcoholic solution, grinding to be semi-dry, standing for a period of time, and calcining to obtain the CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite quantum dot composite material.
As a preferred embodiment of the present invention, the concentration of PbBr 2 in the DMF solution of PbBr 2 is 0.025M; the mass-to-volume ratio of molecular sieve MCM-41 to PbBr 2 in DMF was 0.1 g/800. Mu.l.
As a preferred embodiment of the invention, the concentration of CsBr in the CsBr hydroalcoholic solution is 0.1M, and the hydroalcoholic volume ratio is 1.5:6.5; the mass volume ratio of the molecular sieve MCM-41 to the CsBr aqueous alcohol solution is 0.1 g/1000 mul.
As a preferred embodiment of the present invention, in the step (1), the calcination temperature is 150 to 200℃and the time is 15 to 40 minutes.
In the step (1), the ultrasonic time is 10-20min, the power is not required, and the ultrasonic wave is selected according to actual needs.
As a preferred embodiment of the invention, in the step (1), the drying temperature is 50-80 ℃, the time is not required, and the drying is finished.
As a preferred embodiment of the present invention, in the step (2), the calcination temperature is 150 to 200℃and the time is 20 to 40 minutes.
As a preferred embodiment of the present invention, in the step (2), the calcination is performed after being allowed to stand for 10 minutes.
Compared with the prior art, the invention has the beneficial effects that: the CsPbBr 3/Cs4PbBr6 @MCM-41 composite material has the advantages of high response sensitivity, good reversibility, good repeatability, high response speed and strong controllability of an organic solvent, can be used for detecting the polarity of the organic solvent, and has good detection stability and large application range.
Drawings
Fig. 1 is a flow chart of a preparation process of the perovskite quantum dot composite material.
FIG. 2 is an XRD pattern of perovskite quantum dot composite material and molecular sieve MCM-41 as prepared in example 1.
Fig. 3 is an SEM and EDS plot of SEM of the perovskite quantum dot composite material prepared in example 1.
Fig. 4 is a TEM and EDS plot of a TEM of the perovskite quantum dot composite material prepared in example 1.
Fig. 5 is a high resolution transmission electron microscope image of the perovskite quantum dot composite material prepared in example 1.
Fig. 6 is a 3D waterfall photoluminescence spectrum graph (c), a CIE1931 color coordinate variation graph (a) and a physical graph (b) of the perovskite quantum dot composite material prepared in example 1 in solvents of different polarities at room temperature.
FIG. 7 is a graph showing the fit of the peaks of PL spectra of the perovskite quantum dot composite material obtained in example 1 dispersed in solvents of different polarities. Fig. a is an initial state spectrum of the perovskite quantum dot composite material prepared in example 1, fig. b is a spectrum and a peak splitting treatment graph of the perovskite quantum dot composite material dispersed in n-butanol, fig. c is a spectrum and a peak splitting treatment graph of the perovskite quantum dot composite material dispersed in ethyl acetate, fig. d is a spectrum and a peak splitting treatment graph of the perovskite quantum dot composite material dispersed in ethanol, fig. e is a spectrum and a peak splitting treatment graph of the perovskite quantum dot composite material dispersed in 1, 4-dioxane, and fig. f is a spectrum and a peak splitting treatment graph of the perovskite quantum dot composite material dispersed in acetone.
FIG. 8 is a graph showing the comparison of fluorescence intensity of perovskite quantum dot composite material prepared in example 1 in solvents of different polarities.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples.
Example 1
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) 4mL of a DMF solution of PbBr 2 with the concentration of 0.025M is mixed with 0.5g of molecular sieve MCM-41, the mixture is subjected to ultrasonic treatment for 20min, the sample is dried in a 70 ℃ oven after centrifugation, and finally the sample is transferred into a crucible and is fired in a muffle furnace with the temperature of 200 ℃ for 30min, so that PbBr 2 @MCM-41 is obtained.
(2) Adding 0.107gPbBr 2 @MCM-41 into 4mL of 0.1MCsBr aqueous-alcoholic solution (the volume ratio of the aqueous to the alcoholic is 1.5:6.5), grinding to be semi-dry, placing in the air for 10min, transferring into an alumina crucible, firing in a muffle furnace at 200 ℃ for 30min, and taking out at high temperature to obtain the CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite fluorescent material.
According to FIG. 2, csPbBr 3/Cs4PbBr6 @MCM-41 perovskite quantum dot composite material is successfully synthesized, and according to FIG. 3, three elements of Cs, pb and Br are uniformly distributed in a Si-O skeleton of the MCM, and the atomic ratio of the three elements of Cs, pb and Br is 1:1:3 and 4:1:6, the presence of two phases of CsPbBr 3/Cs4PbBr6 is illustrated.
As can be seen from fig. 4 and fig. 5, cs, pb, br, si, O elements are uniformly distributed, and the atomic ratio of Cs, pb, br is 1:1:3 and 4:1:6, the presence of two phases of CsPbBr 3/Cs4PbBr6 is illustrated. The presence of two lattice fringes can be seen by high resolution transmission electron microscopy, corresponding to the two crystal planes of CsPbBr 3 and Cs 4PbBr6, respectively.
Example 2
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) 4mL of a DMF solution of PbBr 2 with the concentration of 0.025M is mixed with 0.5g of molecular sieve MCM-41, the mixture is subjected to ultrasonic treatment for 10min, the sample is dried in an oven at 80 ℃ after centrifugation, and finally the sample is transferred into a crucible and is fired in a muffle furnace at 150 ℃ for 15min, so that PbBr 2 @MCM-41 is obtained.
(2) Adding 0.107gPbBr 2 @MCM-41 into 4mL of 0.1MCsBr aqueous-alcoholic solution (the volume ratio of the aqueous to the alcoholic is 1.5:6.5), grinding to be semi-dry, placing in the air for 10min, transferring into an alumina crucible, firing in a muffle furnace at 150 ℃ for 40min, and taking out at high temperature to obtain the CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite fluorescent material.
Comparative example 1
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) 4mL of a DMF solution of 0.1M PbBr 2 is mixed with 0.5g of molecular sieve MCM-41, the mixture is subjected to ultrasonic treatment for 20min, the sample is dried in a 70 ℃ oven after centrifugation, and finally the sample is transferred into a crucible and is fired in a muffle furnace at 200 ℃ for 30min, so that PbBr 2 @MCM-41 is obtained.
(2) Then adding the mixture into 4mL of 0.1MCsBr aqueous alcohol solution (the volume ratio of the aqueous alcohol is 1.5:6.5), grinding the mixture to be semi-dry, placing the mixture in air for 10min, transferring the mixture into an alumina crucible, firing the mixture in a muffle furnace at 200 ℃ for 30min, and taking out the mixture at a high temperature to obtain the CsPbBr 3 @MCM-41 perovskite fluorescent material.
Comparative example 2
The preparation method of the perovskite quantum dot composite material comprises the following steps:
4mL of a DMF solution of PbBr 2 with the concentration of 0.025M is mixed with 1mL of a hydroalcoholic solution of 0.1MCsBr (the volume ratio of the hydroalcoholic solution is 1.5:6.5), then the mixture is mixed with 0.5g of molecular sieve MCM-41, the mixture is subjected to ultrasonic treatment for 20min, after centrifugation, the sample is dried in a 70 ℃ oven, finally the sample is transferred to a crucible, and the crucible is fired in a muffle furnace with the temperature of 200 ℃ for 30min, so that the CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite fluorescent material is obtained.
Comparative example 3
The only difference between this comparative example and example 1 is: the molecular sieve MCM-41 is replaced by mesoporous Al 2O3 with the same mass, and the aperture is 18.84nm.
Comparative example 4
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) 4mL of a DMF solution of PbBr 2 with the concentration of 0.025M is mixed with 0.5g of molecular sieve MCM-41, the mixture is subjected to ultrasonic treatment for 20min, the sample is dried in a 70 ℃ oven after centrifugation, and finally the sample is transferred into a crucible and is fired in a muffle furnace with the temperature of 200 ℃ for 30min, so that PbBr 2 @MCM-41 is obtained.
(2) 0.107G of PbBr 2 @MCM-41 is added into 0.8mL of 0.1M CsBr aqueous alcohol solution (the volume ratio of the aqueous alcohol is 1.5:6.5), and the mixture is ground to be half-dry, placed in the air for 10min, then transferred into an alumina crucible, fired in a muffle furnace at 200 ℃ for 30min, and taken out at high temperature to obtain the CsPbBr 3 @MCM-41 perovskite fluorescent material.
Effect example 1
A testing method of perovskite quantum dot composite material in detecting solvent polarity comprises the following steps:
(1) Dispersing 0.03g of perovskite quantum dot composite materials of examples 1-2 and comparative examples 1-4 in 3mL of organic solvent to be detected, measuring a luminescence spectrum under 365nm light irradiation, carrying out Gaussian peak-splitting fitting on the spectrum under 365nm ultraviolet excitation by adopting Origin to obtain a blue light luminescence peak with a wavelength of 460-490nm and a green light luminescence peak with a wavelength of 500-530 nm; the relative intensity values of the blue light luminescence peak and the green light luminescence peak are brought into a linear standard curve, and the polarity of the organic solvent to be detected is calculated; the organic solvent to be detected is an organic solvent with unknown polarity.
(2) Drawing a standard curve: and (3) respectively obtaining the light-emitting spectrum of each material in each organic solvent under 365nm light irradiation and the relative intensity values of a blue light-emitting peak and a green light-emitting peak according to the method of the step (1) by using the organic solvents of dichloromethane, 1-butanol, ethanol, ethyl acetate, 1, 4-dioxane and acetone, and respectively drawing standard curves of polarities of different organic solvents and the relative intensity values of the blue light-emitting peak and the green light-emitting peak of corresponding materials to respectively obtain equations of linear standard curves of each material.
The relative intensity value F of the blue light emission peak and the green light emission peak is f=i B/IG, where I B is the blue light emission peak fluorescence intensity and I G is the green light emission peak fluorescence intensity.
As can be seen from fig. 6 (c), the relative intensity of the luminescence peak near 527nm of the perovskite quantum dot composite material prepared in example 1 gradually increased with the increase of polarity. The change in photoluminescent colour from blue to green can be seen by CIE1931 (see fig. 6 (a)) and the physical diagram (see fig. 6 (b)).
As shown in fig. 7, the change of the relative intensities of the blue light-emitting peak and the green light-emitting peak of the perovskite quantum dot composite material prepared in example 1 with the increase of the polarity can be clearly seen by fitting the spectral peak-splitting, and as can be seen from fig. 8, the intensity ratios of the blue light-emitting peak and the green light-emitting peak of different solvents are counted, and fitting is performed, so as to obtain a curve capable of predicting the polarity of the organic solvent according to the fluorescence intensity ratio, namely a polarity detection model curve: Wherein a 1、A2、X0、dx is a fixed value, a 1＝1.71075,A2＝0.17707,X0＝4.48781,dx =0.17301, f is a relative intensity value of a blue light emission peak and a green light emission peak, and P is a polarity of the organic solvent. From fig. 8, it can be seen that the measured polarity of the organic solvent is very good in fit to the fitted curve. In addition, the invention tests that the composite material prepared in the embodiment 1 is respectively dispersed in absolute ethyl alcohol and ethyl acetate with the polarity of about 4.3, the fluorescence intensity ratio of a blue light luminescence peak to a green light luminescence peak under 365nm ultraviolet light excitation is 1.3052 and 1.3419 respectively, and the relative error of the fluorescence intensity ratio of the two is less than 3%, which shows the reliability of detecting the polarity of the organic solvent.
The materials prepared in example 2 were similar to those prepared in example 1, and all gave the same polarity detection model curves: The CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite fluorescent material can accurately measure the polarity of a solvent to be measured, and the error of the fluorescence intensity ratio of a blue light luminescence peak to a green light luminescence peak of the material prepared in the embodiment 2 dispersed in absolute ethyl alcohol and ethyl acetate is less than 3%, which indicates the reliability of the invention for detecting the polarity of an organic solvent.
The CsPbBr 3 @MCM-41 perovskite fluorescent material prepared in comparative example 1 has no surface defect of Cs 4PbBr6 phase passivation quantum dots, so that the relative intensity of a luminescence peak near 527nm of the prepared CsPbBr 3 @MCM-41 perovskite fluorescent material gradually increases along with the increase of polarity, and the photoluminescence color changes from blue to green, but compared with examples 1-2, the luminescence stability and the luminescence intensity of the material prepared in comparative example 1 are obviously reduced, and the fitting degree of a drawn polarity detection model curve and the accuracy of a test polarity result are poor.
The initial state of the CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite fluorescent material prepared in comparative example 2 shows green luminescence, and the polarity of an organic solvent cannot be detected.
The initial state of the material prepared in comparative example 3 was green luminescence, and the polarity of the organic solvent could not be detected.
The CsPbBr 3 @MCM-41 perovskite fluorescent material prepared in comparative example 4 has no surface defect of Cs 4PbBr6 phase passivation quantum dots, and the photoluminescence color of the organic solvent with different polarities is changed from blue to green, so that the luminescence stability and the luminescence intensity of the material prepared in comparative example 4 are obviously reduced compared with those of examples 1-2, and the fitting degree of a drawn polar detection model curve and the accuracy of a test polar result are poor.
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 scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (5)
1. The application of the perovskite quantum dot composite material in the polarity detection of the organic solvent is characterized in that the perovskite quantum dot composite material is CsPbBr 3/Cs4PbBr6 @MCM-41 composite material; csPbBr 3/Cs4PbBr6 is loaded in the pore canal of the MCM-41 molecular sieve;
The preparation method of the perovskite quantum dot composite material comprises the following steps:
(1) Mixing a DMF solution of PbBr 2 with a molecular sieve MCM-41, sequentially carrying out ultrasonic treatment, drying and calcining to obtain PbBr 2 @MCM-41;
(2) Adding PbBr 2 @MCM-41 into a CsBr hydroalcoholic solution, grinding to be semi-dry, standing for a period of time, and calcining to obtain a CsPbBr 3/Cs4PbBr6 @MCM-41 perovskite quantum dot composite material;
The concentration of PbBr 2 in the DMF solution of PbBr 2 is 0.025M; the mass volume ratio of the molecular sieve MCM-41 to the DMF solution of PbBr 2 is 0.1g:800 mul;
the concentration of CsBr in the CsBr hydroalcoholic solution is 0.1M, and the hydroalcoholic volume ratio is 1.5:6.5; the mass volume ratio of the molecular sieve MCM-41 to the CsBr aqueous alcohol solution is 0.1 g/800 μl.
2. The use according to claim 1, comprising the steps of:
Dispersing the perovskite quantum dot composite material in an organic solvent to be detected, and carrying out peak-splitting fitting on a fluorescence spectrum excited by 365nm ultraviolet light to obtain fluorescence intensities of a blue light luminescence peak and a green light luminescence peak; the relative intensity values of the blue light luminescence peak and the green light luminescence peak are brought into a polar detection model curve, and the polarity of the organic solvent to be detected is calculated;
The relative intensity value f=i B/IG of the blue light emission peak and the green light emission peak, wherein I B is the fluorescence intensity of the blue light emission peak, and I G is the fluorescence intensity of the green light emission peak.
3. The use according to claim 2, wherein the relative intensity values of the blue light emission peak and the green light emission peak of the perovskite quantum dot composite material in different organic solvents are numerically fitted to the polarity of the organic solvents to obtain the equation of the polarity detection model curve as follows: Wherein a 1、A2、X0、dx is a fixed value, a 1＝1.71075,A2＝0.17707,X0＝4.48781,dx =0.17301, f is a relative intensity value of a blue light emission peak and a green light emission peak, and P is a polarity of the organic solvent.
4. The use according to claim 1, wherein in step (1), the calcination temperature is 150 to 200 ℃ for 15 to 40min.
5. The use according to claim 1, wherein in step (2), the calcination temperature is 150-200 ℃ for 20-40min.
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