CN108774520B - Preparation method of cesium-lead-bromine quantum dots based on liquid-phase laser irradiation of halogen perovskite - Google Patents

Preparation method of cesium-lead-bromine quantum dots based on liquid-phase laser irradiation of halogen perovskite Download PDF

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CN108774520B
CN108774520B CN201810253031.6A CN201810253031A CN108774520B CN 108774520 B CN108774520 B CN 108774520B CN 201810253031 A CN201810253031 A CN 201810253031A CN 108774520 B CN108774520 B CN 108774520B
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邹友生
董宇航
曾海波
韩泽尧
李举彬
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Nanjing University of Science and Technology
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Abstract

The invention discloses a preparation method of cesium-lead-bromine quantum dots based on liquid-phase laser irradiation halogen perovskite. The all-inorganic halogen perovskite is a novel fluorescent nano material with relatively low toxicity, low cost and high quality, and has wide application prospect in the fields of illumination, display, communication, sensing, biological imaging, detection and the like. The method adopts a liquid-phase laser irradiation method, takes cesium lead bromide powder as a raw material, takes oleylamine and oleic acid as ligands, and synthesizes the cesium lead bromide quantum dots with a single-phase structure, good crystallinity and uniform appearance and size in an organic solvent. Compared with the existing preparation method of the cesium-lead-bromine nanomaterial, the method provided by the invention has the advantages of wide raw material source, easiness in operation, mild experimental conditions, no need of heating and protective gas, high repeatability and the like.

Description

Preparation method of cesium-lead-bromine quantum dots based on liquid-phase laser irradiation of halogen perovskite
Technical Field
The invention relates to the technical field of preparation of all-inorganic halogen perovskite, in particular to a preparation method of cesium lead bromine quantum dots based on liquid-phase laser irradiation of halogen perovskite.
Background
The semiconductor fluorescent material has wide application in the dual-purpose fields of illumination, display, communication, sensing, biological imaging and the like. In recent years, with the advent of novel perovskite solar cells, a novel semiconductor material, namely, all-inorganic halogen perovskite, becomes a research hotspot in the field of material science. The material has been reported to have excellent light-emitting characteristics, and simultaneously, the visible light full-wave-band coverage can be realized through halogen ion regulation, so that the material is expected to become a core material in the next generation of LED.
At present, a few reports on the synthesis method of the all-inorganic halogen perovskite quantum dot exist. Lace dream et al (ACS appl.mater.inter.2017,9,26556) dissolve lead bromide and cesium bromide in DMSO, inject the DMSO solution, oleylamine and oleic acid together into a toluene solution, stir continuously, and centrifuge dry to obtain CsPbBr3/Cs4PbBr6Double perovskite structure, improved CsPbBr3The quantum dots have thermal stability and are expected to be applied to multiple anti-counterfeiting aspects. Chinese patent (201610986787.2) disclosesThe preparation method of the cesium-lead-bromine quantum dots adopts a thermal injection method, uses oleic acid and octadecene as coordination and coordination solvents, and utilizes a nitrogen protection and heating method to generate cesium-lead-bromine quantum dot colloids, and the obtained all-inorganic cesium-lead-bromine colloids have good dispersibility and uniform particles and high luminous efficiency. Chinese patent (201610066113.0) discloses a method for synthesizing metal halide perovskite quantum dots with high luminous efficiency light color gamut by a low temperature solution method, which comprises the steps of preserving heat of a reaction solvent at a certain temperature, stirring, rapidly injecting metal halide precursor salt into the reaction solvent, and finally cooling to room temperature by water to obtain the metal halide perovskite quantum dots with high luminous efficiency. Chinese patent (201610067793.8) discloses a synthetic CsPbX3The method for preparing the inorganic perovskite nanosheet adopts a high-temperature hot injection method, and the metal halide precursor reacts in an oil system under the protection of inert gas to generate the perovskite nanosheet.
However, most of the reported methods for preparing cesium-lead-bromine quantum dots are normal-temperature supersaturated precipitation methods and high-temperature thermal injection methods, and the precursor is mostly prepared by cesium bromide, lead bromide or other metal salts, so that the reaction precursor needs to be accurately regulated and controlled. At present, no report of a preparation method for preparing all-inorganic halogen perovskite cesium lead bromide quantum dots based on liquid-phase laser irradiation is found.
Disclosure of Invention
The invention aims to provide a preparation method of a cesium-lead-bromine quantum dot based on liquid-phase laser irradiation halogen perovskite.
The technical solution for realizing the purpose of the invention is as follows: a cesium lead bromine quantum dot with a single-phase structure, good crystallinity and uniform and controllable morphology is prepared by irradiating cesium lead bromine powder immersed in a solution with liquid-phase laser under a mild condition, and the method specifically comprises the following steps:
step 1, adding cesium-lead-bromine powder, an organic solvent, oleylamine and oleic acid into a container, and uniformly stirring the solution by using a magnetic stirrer; the added organic solvent is toluene, the mass ratio of cesium lead bromide powder to toluene is 1:200-1:2200, the volume ratio of oleylamine to toluene is 1:100-1:400, and the volume ratio of oleylamine to oleic acid is 1:0-1: 1.
And 2, adjusting the optical path, laser energy and frequency of the laser, and irradiating the solution for a certain time. The method specifically comprises the following steps: and adjusting the optical path of the laser to enable the laser to vertically enter the center of the liquid level, wherein the laser wavelength is 532nm, the frequency is 10Hz, the energy is 100-400mJ, and the irradiation time is 10-40 min.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation, and taking supernatant liquor. Measuring a flocculating agent with the volume twice that of the solvent, fully mixing the flocculating agent with the supernatant liquid, and centrifuging. The flocculant is ethyl acetate or acetone, the centrifugation speed is 8000-10000rpm, and the centrifugation time is 1-5 min.
And 4, removing the supernatant, and dispersing the precipitate into a certain amount of nonpolar organic solvent to obtain the halogen perovskite cesium lead bromide quantum dots. The nonpolar organic solvent is n-hexane, n-octane or toluene, and the volume of the solvent is 1-3 mL.
Compared with the prior art, the invention has the following remarkable advantages: the invention uses non-focused laser beam to irradiate perovskite powder to generate nano-scale perovskite particles, and quantum dots with uniform appearance and size are obtained through ligand regulation and growth, the required conditions are mild, and no protective gas is generated; the shape, size and phase structure of the adopted cesium-lead-bromine powder have no influence on the shape, size and phase structure of a final product, the source of raw materials is wide, the limitation is less, and the synthesis steps are simple; the obtained quantum dots have high purity and high repeatability.
Drawings
FIG. 1 is an SEM image of cesium lead bromide powder as a raw material in example 1 of the present invention.
FIG. 2 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 1 of the present invention.
FIG. 3 is a high resolution TEM image of cesium lead bromide quantum dots as the product prepared in example 1 of the present invention.
Fig. 4 is a PL diagram and a physical diagram of the cesium lead bromide quantum dot product prepared in example 1 of the present invention.
Fig. 5 is an XRD pattern of cesium lead bromide quantum dots as a product prepared in example 1 of the present invention.
FIG. 6 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 2 of the present invention.
FIG. 7 is a PL diagram of cesium lead bromide quantum dots as products prepared in example 2 of the present invention.
FIG. 8 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 3 of the present invention.
FIG. 9 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 4 of the present invention.
FIG. 10 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 5 of the present invention.
FIG. 11 is a TEM image of cesium lead bromide quantum dots as a product prepared in example 6 of the present invention.
Detailed Description
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in a solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding cesium-lead-bromine powder, an organic solvent, oleylamine and oleic acid into a glass container, and uniformly stirring the solution by using a magnetic stirrer; the added organic solvent is toluene, the mass ratio of cesium lead bromide powder to toluene is 1:200-1:2200, the volume ratio of oleylamine to toluene is 1:100-1:400, and the volume ratio of oleylamine to oleic acid is 1:0-1: 1.
And 2, adjusting the optical path, laser energy and frequency of the laser, and irradiating the solution for a certain time. The method specifically comprises the following steps: and adjusting the optical path of the laser to enable the laser to vertically enter the center of the liquid level, wherein the laser wavelength is 532nm, the frequency is 10Hz, the energy is 100-400mJ, and the irradiation time is 10-40 min.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation, and taking supernatant liquor. Measuring a flocculating agent with the volume twice that of the solvent, fully mixing the flocculating agent with the supernatant liquid, and centrifuging. The flocculant is ethyl acetate or acetone, the centrifugation speed is 8000-10000rpm, and the centrifugation time is 1-5 min.
And 4, removing the supernatant, and dispersing the precipitate into a certain amount of nonpolar organic solvent to obtain the halogen perovskite cesium lead bromide quantum dots. The nonpolar organic solvent is n-hexane, n-octane or toluene, and the volume of the solvent is 1-3 mL.
The invention utilizes non-focused laser beam to irradiate perovskite powder to generate nano-scale perovskite particles, and the nano-scale perovskite particles are grown by ligand regulation to obtain quantum dots with uniform appearance and size, the required conditions are mild, and no protective gas is generated.
The present invention will be described in further detail with reference to examples.
Example 1
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.012g of cesium lead bromide powder, 30mL of toluene, 100 mu L of oleylamine and 100 mu L of oleic acid into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by adopting a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 40min using a laser wavelength of 532nm, energy of 400mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube, centrifuging at 8000rpm, and taking supernatant. 60mL of ethyl acetate was mixed well with the supernatant and centrifuged at 10000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 2mL of n-hexane to obtain the cesium lead bromide quantum dot.
SEM characterization of the raw materials used in the examples As shown in FIG. 1, the cesium lead bromide powder has irregular morphology and a size of 1 μm. The prepared product is subjected to TEM, high-resolution TEM, PL and XRD characterization and analysis, as shown in figures 2, 3, 4 and 5, and the result shows that uniform cesium-lead-bromine quantum dots with morphology and size can be obtained according to the process parameters of example 1. TEM shows that the size of the cesium-lead-bromine quantum dots is about 15 nm. The high-resolution TEM shows that the single cesium-lead-bromine quantum dot has ultrahigh crystallinity and few internal defects. The PL luminescence peak is located at 514nm, and cesium lead bromide quantum dots dispersed in n-hexane emit bright green under an ultraviolet lamp. The XRD spectrum only shows two characteristic peaks of (100) and (200) without other miscellaneous peaks, which shows that the cesium-lead bromide quantum dots have uniform morphology and size and have good orientation after being dripped and dried on a silicon wafer.
Example 2
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.012g of cesium lead bromide powder, 30mL of toluene and 100 mu L of oleylamine into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by using a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 30min with a laser wavelength of 532nm, energy of 200mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation at 10000rpm, and taking supernatant liquor. 60mL of ethyl acetate was mixed well with the supernatant and centrifuged at 10000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 3mL of n-hexane to obtain the cesium lead bromide quantum dots.
The prepared product is subjected to TEM and PL characterization, as shown in FIGS. 6 and 7, and the result shows that cesium-lead-bromine quantum dots with uniform morphology and size can be obtained according to the process parameters of example 2. TEM shows that cesium-lead-bromine quantum dots with uniform morphology and a size of about 20nm can be obtained according to the process parameters of the embodiment 2, and the PL luminescence peak is located at 514 nm.
Example 3
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.048g of cesium-lead-bromine powder, 10mL of toluene, 100 mu L of oleylamine and 50 mu L of oleic acid into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by using a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 10min with a laser wavelength of 532nm, energy of 300mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation at 9000rpm, and taking supernatant. 20mL of ethyl acetate was mixed well with the supernatant and centrifuged at 10000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 1mL of n-hexane to obtain the cesium-lead-bromine quantum dot.
The product prepared was analyzed by TEM characterization as shown in fig. 8. The TEM result shows that the cesium-lead-bromine quantum dots with uniform morphology and the size of about 10nm can be obtained according to the process parameters of the embodiment 3.
Example 4
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.096g of cesium lead bromide powder, 40mL of toluene, 50 muL of oleylamine and 50 muL of oleic acid into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by using a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 40min using a laser wavelength of 532nm, energy of 400mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation at 10000rpm, and taking supernatant liquor. 80mL of ethyl acetate was mixed well with the supernatant and centrifuged at 10000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 3mL of n-hexane to obtain the cesium lead bromide quantum dots.
The product prepared was subjected to TEM as shown in figure 9. The TEM result shows that the cesium-lead-bromine quantum dots with uniform morphology and the size of about 10nm can be obtained according to the process parameters of the embodiment 4.
Example 5
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.012g of cesium lead bromide powder, 20mL of toluene, 50 muL of oleylamine and 50 muL of oleic acid into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by adopting a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 10min with a laser wavelength of 532nm, energy of 400mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation at 10000rpm, and taking supernatant liquor. 40mL of ethyl acetate was mixed well with the supernatant and centrifuged at 8000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 1mL of n-hexane to obtain the cesium-lead-bromine quantum dot.
The product prepared was subjected to TEM as shown in figure 10. The TEM result shows that the cesium-lead-bromine quantum dots with uniform morphology and the size of about 15nm can be obtained according to the process parameters of the embodiment 5.
Example 6
The cesium-lead-bromine quantum dots with single-phase structures, good crystallinity and uniform and controllable appearance are prepared under mild conditions by irradiating cesium-lead-bromine powder immersed in the solution with liquid-phase laser. The method specifically comprises the following steps:
step 1, adding 0.024g of cesium lead bromide powder, 30mL of toluene and 50 mu L of oleylamine into a long glass test tube, vertically placing the long glass test tube, and uniformly stirring the solution by adopting a magnetic stirrer;
and 2, adjusting the optical path of the laser to enable the pulse laser beam to be parallel to the long test tube, to be incident at the center of the test tube opening and to be irradiated to the center of the liquid level. The solution was irradiated for 20min with a laser wavelength of 532nm, energy of 100mJ and frequency of 10 Hz.
And 3, after the irradiation is finished, transferring the solution into a centrifugal tube for centrifugation at 10000rpm, and taking supernatant liquor. 60mL of ethyl acetate was mixed well with the supernatant and centrifuged at 9000 rpm.
And 4, removing the supernatant, and dispersing the precipitate into 1mL of n-hexane to obtain the cesium-lead-bromine quantum dot.
The product prepared was subjected to TEM as shown in fig. 11. The TEM result shows that the cesium-lead-bromine quantum dots with uniform morphology and the size of about 20nm can be obtained according to the process parameters of the embodiment 4.

Claims (5)

1. A preparation method of cesium-lead-bromine quantum dots based on liquid-phase laser irradiation halogen perovskite is characterized by comprising the following steps:
step 1, adding cesium-lead-bromine powder, an organic solvent, oleylamine and oleic acid into a container, and uniformly stirring the solution by using a magnetic stirrer;
step 2, adjusting the optical path, laser energy and frequency of the laser, and irradiating the solution for a certain time;
step 3, after the irradiation is finished, transferring the solution into a centrifuge tube for centrifugation, and taking supernatant liquor; measuring a flocculating agent with the volume twice that of the solvent, fully mixing the flocculating agent with the supernatant liquor, and centrifuging;
and 4, removing the supernatant, and dispersing the precipitate into a certain amount of nonpolar organic solvent to obtain the halogen perovskite cesium lead bromide quantum dots.
2. The preparation method of the cesium lead bromine quantum dots based on the liquid-phase laser irradiation halogen perovskite, which is characterized in that the organic solvent added in the step 1 is toluene, the mass ratio of cesium lead bromine powder to toluene is 1:200-1:2200, the volume ratio of oleylamine to toluene is 1:100-1:400, and the volume ratio of oleylamine to oleic acid is 1:0-1: 1.
3. The preparation method of cesium lead bromide quantum dots based on liquid phase laser irradiation as claimed in claim 1, wherein in step 2, the laser path is adjusted to make laser vertically incident to the center of the liquid surface, the laser wavelength is 532nm, the frequency is 10Hz, the energy is 100-400mJ, and the irradiation time is 10-40 min.
4. The preparation method of cesium lead bromide quantum dots based on liquid phase laser irradiation of halogen perovskite according to claim 1, wherein the flocculant in step 3 is ethyl acetate or acetone, the centrifugation speed is 8000-10000rpm, and the centrifugation time is 1-5 min.
5. The preparation method of cesium lead bromide quantum dots based on liquid-phase laser irradiation of halogen perovskite according to claim 1, wherein the nonpolar organic solvent in step 4 is n-hexane, n-octane or toluene, and the volume of the solvent is 1-3 mL.
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