CN108753284B - High-fluorescence red light emission Mn: CsPbCl3Preparation method of nano-cluster - Google Patents

High-fluorescence red light emission Mn: CsPbCl3Preparation method of nano-cluster Download PDF

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CN108753284B
CN108753284B CN201810381888.6A CN201810381888A CN108753284B CN 108753284 B CN108753284 B CN 108753284B CN 201810381888 A CN201810381888 A CN 201810381888A CN 108753284 B CN108753284 B CN 108753284B
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cspbcl
nano
cluster
red light
octadecene
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CN108753284A (en
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张颖
李思
解仁国
汪大洋
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Jilin University
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    • C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
    • C09K11/664—Halogenides
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
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Abstract

The invention relates to high-fluorescence red light emission Mn: CsPbCl3A preparation method of nanoclusters belongs to the technical field of semiconductor nanomaterial preparation, and comprises the steps of firstly, weighing lead chloride, oleic acid, oleylamine and octadecene, placing the weighed materials in a three-necked bottle, vacuumizing the bottle at 120 ℃, adding trioctylphosphine under the protection of nitrogen, and dissolving the materials at 150 ℃ to form a mixed solution; then, cooling the mixed solution to room temperature, injecting a cesium oleate solution, and reacting at room temperature to obtain CsPbCl3Nanoclusters; finally, CsPbCl was added3Purifying the nano-clusters, transferring the nano-clusters into a mortar, adding manganese salt, and grinding to obtain Mn, CsPbCl3A nanocluster. CsPbCl serving as Mn prepared by the invention3Realizes the doping of Mn element in CsPbCl for the first time3In the nano cluster, the red light emitting efficiency is higher. The whole reaction is simple to operate, raw materials are easy to obtain, a large amount of raw materials can be synthesized, and the product has a wide application prospect.

Description

High-fluorescence red light emission Mn: CsPbCl3Preparation method of nano-cluster
Technical Field
The invention belongs to the technical field of semiconductor nano material preparation, and relates to high-fluorescence red light emission Mn: CsPbCl3A method for preparing nanoclusters.
Background
Magic size nanoclusters (magic size clusters) are generally defined as nanocrystals with a crystal structure size of less than 2nm with a full shell structure of the corresponding crystalline material. Because of this complete full shell structure, magic-sized nanoclusters are thermodynamically more stable than clusters that are slightly smaller or larger than them without a full shell structure. The magic size nanocluster widens the size range of the nanocrystal, provides a model platform for the physicochemical research of the semiconductor nanocrystal with the size, can better understand the evolution process of physicochemical properties of a substance in the process of converting from molecular size to nanoscale, and has certain research significance in basic research and practical application.
The transition metal doped semiconductor nanocrystal is characterized in that optically or magnetically active doped ions are introduced into the semiconductor nanocrystal. By adjusting the size of the II-VI and III-V group semiconductor nanocrystals and doping the transition metal, the semiconductor nanocrystals have stable visible-near infrared emission spectra, and moreover, the transition metal doped semiconductor nanocrystals have the characteristics of high thermal and environmental stability, longer excited state life, large Stokes shift, effective avoidance of self-absorption of luminescent materials and the like, so that the application range of the semiconductor nanocrystals is obviously expanded. As early as 1983, doped nanocrystals were reported, and the fluorescence lifetime decreased by 5 orders of magnitude after Mn doping in ZnS nanocrystals by the Becker group, and since this time, interest in doped nanocrystals has continued to grow, although it was later demonstrated that the observed decay in fluorescence lifetime is indeed due to the effect of defect emission.
Mn2+Is one of the most important doped transition metals, and is often doped in II-VI group and multi-component semiconductor nanocrystals as a means for introducing new functions, such as Mn: ZnSe, Mn: CuInS2Mn: CdS/ZnS, etc., however, there are many problems to be further investigated. On one hand, most of the fluorescence emitted by the manganese-doped nanocrystal is yellow orange light, the emission peak position of Mn-doped emission is 580-600 nm, and only a few phenomena capable of being doped into red light exist, and if the manganese-doped emission can be further adjusted to the red light, the red light is one of three primary colors of color light, so that the manganese-doped nanocrystal has great application potential in the fields of displays and illumination; on the other hand, the smaller the doped host nanocrystal size is, the stronger the quantum confinement is, the interaction between the doping and the host nanocrystal can generate huge magneto-optical and magneto-electric responses, and the method has important application in products such as spin-emitting semiconductors (spin-LEDs) and Faraday optical isolators, but because the small-size nanocrystal has strong rejection to the doping, the manganese-doped magic-size nanoclusters are difficult to obtain.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the problems in the background technology and provides high-fluorescence red light emission Mn: CsPbCl for the first time3A method for preparing nanoclusters.
The new preparation method provided by the invention is to prepare the product at low temperaturePrepared Mn: CsPbCl3The nano-cluster has uniform size and good monodispersity; wherein the emission peak position of Mn doping emission can reach 628nm, and the fluorescence efficiency can reach 60%. Moreover, the feeding of manganese salt is greatly reduced in the reaction, the reaction cost is reduced, and the method is suitable for industrial large-scale production.
The technical problem is solved by the following technical scheme:
high-fluorescence red light emission Mn: CsPbCl3Firstly, weighing lead chloride, oleic acid, oleylamine and octadecene, placing the weighed materials in a three-necked bottle, vacuumizing the bottle at 120 ℃, adding trioctylphosphine under the protection of nitrogen, and dissolving the trioctylphosphine at 150 ℃ to form a mixed solution, wherein 2.5mL of oleic acid, 2.5mL of oleylamine, 10mL of octadecene and 2.5mL of trioctylphosphine are used for each mmol of lead chloride; then, the mixed solution is cooled to room temperature, and cesium oleate solution with the concentration of 0.2M is injected into the mixed solution to react for 1 hour at room temperature to obtain CsPbCl3Nanoclusters using 1ml of 0.2M cesium oleate per mmol lead chloride; finally, CsPbCl was added3Centrifugally purifying the nano-cluster in a centrifugal machine with 8000rpm, transferring the nano-cluster into a mortar, adding manganese salt, and grinding to obtain Mn, CsPbCl3A nanocluster.
The manganese salt is preferably anhydrous manganese chloride or tetrahydrate manganese chloride solid powder, and manganese element in the manganese salt and CsPbCl3The molar ratio of the lead element in the nanocluster is preferably 0.25-1; the temperature during milling is preferably not more than 30 ℃ and the ambient relative humidity is preferably not more than 30%.
The cesium oleate solution can be prepared by the following method: weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing in a three-necked bottle, vacuumizing at 120 ℃, and heating to 150 ℃ under the protection of nitrogen to dissolve to obtain a 0.2M cesium oleate solution.
Has the advantages that:
the invention grinds manganese salt and CsPbCl by a grinding method3Nano cluster, under the condition of low temperature, obtaining high fluorescence red light emission Mn: CsPbCl3A nanocluster. The nano-cluster has good monodispersity and stronger red light emission, and the fluorescence quantum efficiency can reach 60 percent at most. The whole reaction is simple to operate, raw materials are easy to obtain, and the product can be synthesized in a large quantityHas wide application prospect.
Description of the drawings:
FIG. 1 shows the Mn: CsPbCl prepared in example 1 of the present invention3Absorption spectrum of nanoclusters.
FIG. 2 shows CsPbCl prepared differently for examples 1, 2, 3 as a function of manganese chloride charge3Emission spectrum of nanoclusters.
FIG. 3 is a high fluorescent red light emitting Mn: CsPbCl prepared in example 4 of the present invention3Photo of nanoclusters under uv lamp.
FIG. 4 is a high fluorescent red light emitting Mn: CsPbCl prepared in example 5 of the present invention3Photograph under ultraviolet lamp with nanoclusters dispersed in n-hexane.
FIG. 5 shows CsPbCl as Mn prepared in example 6 of the present invention3XRD diffractogram of nanocluster.
Detailed Description
Example 1:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine and 6mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 1.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 0.6mL of cesium oleate solution is injected, and the reaction is carried out at the room temperature for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.12mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.06mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The absorption spectrum is shown in FIG. 1, and the emission spectrum is shown in FIG. 2 (PL 2).
Example 2:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine and 6mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 1.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 0.6mL of cesium oleate solution is injected, and the reaction is carried out at the room temperature for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.12mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.03mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The absorption spectrum was the same as that of example 1, and the emission spectrum was as shown in FIG. 2 (PL 1).
Example 3:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine and 6mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 1.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 0.6mL of cesium oleate solution is injected, and the reaction is carried out at the room temperature for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.12mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.12mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The absorption spectrum was the same as that of example 1, and the emission spectrum was as shown in FIG. 2 (PL 3).
Example 4:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 0.2mmol of lead chloride, 0.5mL of oleic acid, 0.5mL of oleylamine and 2mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 0.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 0.2mL of cesium oleate solution is injected, and the reaction is carried out at the room temperature for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.04mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.02mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The photograph under UV light is shown in FIG. 3.
Example 5:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 3mmol of lead chloride, 7.5mL of oleic acid, 7.5mL of oleylamine and 30mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 7.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 3mL of cesium oleate solution is injected, and the room temperature reaction is carried out for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.6mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.3 mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The prepared Mn: CsPbCl3The nanoclusters were dispersed in n-hexane and irradiated with an ultraviolet lamp, and the photograph was as shown in FIG. 4 (red).
Example 6:
firstly, weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing the cesium carbonate, the oleic acid and the octadecene into a three-necked bottle, vacuumizing at 120 ℃, heating to 150 ℃ under the protection of nitrogen, dissolving to form 0.2M cesium oleate solution, and cooling to room temperature for later use;
then, 0.6mmol of lead chloride, 1.5mL of oleic acid, 1.5mL of oleylamine and 6mL of octadecene are weighed and placed in a three-necked bottle, vacuumizing is carried out at 120 ℃, 1.5mL of trioctylphosphine is added under the protection of nitrogen, the mixture is dissolved at 150 ℃ to form a mixed solution, an ice water bath is cooled to room temperature, 0.6mL of cesium oleate solution is injected, and the reaction is carried out at the room temperature for 1h to obtain CsPbCl3Nanoclusters;
finally, CsPbCl was added3Directly placing the mother liquor of the nano-cluster into a centrifuge to centrifuge at 8000rpm for 5min for purification, removing the supernatant, and obtaining 0.12mmol CsPbCl3Transferring the perovskite nanocrystalline precipitate to a mortar, and adding 0.06mmol of anhydrous MnCl2Grinding to obtain the high-fluorescence red light emission Mn: CsPbCl3A nanocluster. The XRD diffraction pattern is shown in figure 5.

Claims (3)

1. High-fluorescence red light emission Mn: CsPbCl3Firstly, weighing lead chloride, oleic acid, oleylamine and octadecene, placing the weighed materials in a three-necked bottle, vacuumizing the bottle at 120 ℃, adding trioctylphosphine under the protection of nitrogen, and dissolving the trioctylphosphine at 150 ℃ to form a mixed solution, wherein 2.5mL of oleic acid, 2.5mL of oleylamine, 10mL of octadecene and 2.5mL of trioctylphosphine are used for each mmol of lead chloride; then, the mixed solution is cooled to room temperature, and cesium oleate solution with the concentration of 0.2M is injected into the mixed solution to react for 1 hour at room temperature to obtain CsPbCl3Nanoclusters using 1ml of 0.2M cesium oleate per mmol lead chloride; finally, CsPbCl was added3Centrifugally purifying the nano-cluster in a centrifugal machine with 8000rpm, transferring the nano-cluster into a mortar, adding manganese salt, and grinding to obtain Mn, CsPbCl3A nanocluster.
2. The highly fluorescent red light emitting Mn: CsPbCl according to claim 13The preparation method of the nano-cluster is characterized in that the manganese salt is anhydrous manganese chloride or tetrahydrate manganese chloride solid powder, and manganese element in the manganese salt and CsPbCl3The molar ratio of the lead element in the nano-cluster is 0.25-1;the temperature during grinding is not more than 30 ℃, and the relative humidity of the environment is not more than 30%.
3. A highly fluorescent red emitting Mn: CsPbCl according to claim 1 or 23The preparation method of the nanocluster is characterized in that the cesium oleate solution can be prepared by the following method: weighing 2mmol of cesium carbonate, 2.5mL of oleic acid and 17.5mL of octadecene, placing in a three-necked bottle, vacuumizing at 120 ℃, and heating to 150 ℃ under the protection of nitrogen to dissolve to obtain a 0.2M cesium oleate solution.
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CN115029134A (en) * 2022-05-27 2022-09-09 广西大学 Efficient Mn-doped CsPbCl based on aluminum chloride auxiliary preparation 3 Method for producing nanocrystals

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