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CN-121975516-A - High stability Cs2ZnCl4:Cu+Microwave-assisted one-step synthesis method and application of nano luminescent material

CN121975516ACN 121975516 ACN121975516 ACN 121975516ACN-121975516-A

Abstract

A microwave-assisted one-step synthesis method and application of a high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material. The synthesis method comprises the steps of weighing Cs 2 H 3 O 2 、ZnCl 2 , cuCl and trioctylphosphine oxide, adding oleic acid, oleylamine and 1-octadecene, stirring uniformly to prepare a mixture, placing the mixture into a microwave reactor, heating the mixture to complete the synthesis reaction under the stirring condition, quenching the reaction by using an ice water bath, and washing the reaction product to obtain the Cs 2 ZnCl 4 :Cu + nanometer luminescent material with high stability. The invention has the advantages that the microwave-assisted synthesis technology is adopted, all the reaction raw materials and the auxiliary agent are added into the reaction container in one step, and the product synthesis can be realized under the environmental condition. The obtained Cs2ZnCl4 Cu+ nano luminescent material has a nano crystalline structure, emits bright green light under the excitation of ultraviolet light, and has a photoluminescence quantum yield (PLQY) as high as 35.3 percent. The obtained product has good crystallinity, high stability, environmental friendliness and excellent and stable luminescence performance. The material can be applied to the fields of nondestructive detection, illumination display, anti-counterfeiting, photoelectric detection and the like.

Inventors

  • Geng Donglian
  • LI JINHENG
  • LI JINGTAO
  • CHEN JUNRU

Assignees

  • 中国民航大学

Dates

Publication Date
20260505
Application Date
20260116

Claims (7)

  1. 1. A microwave-assisted one-step synthesis method of a high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material is characterized by comprising the following steps in sequence: 1) Weighing Cs 2 H 3 O 2 、ZnCl 2 , cuCl and trioctylphosphine oxide serving as reaction raw materials according to a proportion, placing the mixture in a container, then adding oleic acid, oleylamine and 1-octadecene serving as surfactants according to a proportion, and uniformly stirring to prepare a mixture; 2) Placing a magnetic stirrer in a container, sealing the container, placing the container and the mixture in the container in a microwave reactor, heating the container and the mixture under stirring until the synthesis reaction is completed, and quenching the reaction by using an ice water bath; 3) And washing the reaction product with an organic solvent and dispersing the reaction product in n-hexane to obtain the high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material which emits bright green light under the excitation of ultraviolet light.
  2. 2. The microwave-assisted one-step synthesis method of the high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material according to claim 1, wherein in the step 1), the stoichiometric ratio of the reaction raw materials is Cs + ：(Zn 2+ +Cu + ) =1:2, the doping concentration of Cu + is 2-30%, the stoichiometric ratio of trioctylphosphine oxide to Cs+ is (0.5-2): 2, the amount of Cs+ added is 1-4 mL for each 0.2mmol of Cs+, the stoichiometric ratio of oleic acid/oleylamine is (0.25-4): 1, and the amount of C+ added is 1-3 mL for each 0.2mmol of Cs+.
  3. 3. The microwave-assisted one-step synthesis method of the high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material according to claim 2, wherein the doping concentration of Cu + is 5%, the stoichiometric ratio of trioctylphosphine oxide to Cs+ is 1:2, the amount of oleic acid is 4mL when each 0.2mmol of Cs+ is added, the stoichiometric ratio of oleic acid to oleylamine is 4:1, and the amount of 1-octadecene is 2mL when each 0.2mmol of Cs+ is added.
  4. 4. The microwave-assisted one-step synthesis method of high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material according to claim 1, wherein in step 2), the temperature of the synthesis reaction is 60-160 ℃ and the time is 5-30 min in a microwave reactor.
  5. 5. The microwave-assisted one-step synthesis method of high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material according to claim 4, wherein the temperature of the synthesis reaction is 120 ℃ and the time is 20min.
  6. 6. The microwave-assisted one-step synthesis method of the high-stability Cs 2 ZnCl 4 :Cu + nanometer luminescent material according to claim 1, wherein in the step 3), ethyl acetate and n-hexane are selected as the organic solvent, and the washing method is that the ethyl acetate is washed three times and the n-hexane is washed once.
  7. 7. Use of the Cs 2 ZnCl 4 :Cu + nano-luminescent material with high stability according to any one of claims 1 to 6 in the fields of nondestructive inspection, illumination display, anti-counterfeiting and photoelectric detection.

Description

Microwave-assisted one-step synthesis method and application of high-stability Cs 2ZnCl4:Cu+ nanometer luminescent material Technical Field The invention belongs to the technical field of inorganic luminescent material synthesis, and particularly relates to a microwave-assisted one-step synthesis method and application of a high-stability Cs 2ZnCl4:Cu+ nanometer luminescent material. Background Although the lead halide perovskite nano material has excellent photoelectric characteristics, the inherent lead toxicity and phase separation problem caused by ion migration severely restrict the commercialized application prospect. The low-dimensional lead-free substitute material such as a copper-doped zinc halide compound with self-trapping state exciton luminescence property has potential advantages due to the characteristics of structural adjustability, stability enhancement and the like, wherein Cs 2ZnCl4 and the like are favorable for efficient doping of copper ions and inhibiting exciton diffusion loss by virtue of an isolated tetrahedral coordination geometry structure. However, the existing nano material synthesis methods, such as a thermal injection method and a ligand-assisted reprecipitation method, still have key limitations such as oxidative degradation caused by long reaction time, influence on optical consistency due to non-uniform morphology, low heat transfer efficiency, and blockage of crystallinity regulation and control. The root of these problems is mainly the dynamic barrier faced by insufficient thermal management and defect repair during synthesis. Although microwave-assisted synthesis techniques can provide potential advantages for material preparation by volumetric rapid heating, related studies have not been adequate in lead-free metal halide systems, particularly in the context of externally doped compositions requiring precise doping and defect control. The technical blank makes it difficult to achieve an effective balance between synthesis efficiency and material stability, thereby impeding the development of nanomaterials with high optical properties and long-term environmental stability, and limiting the progress towards commercial photoelectric applications. Therefore, there is an urgent need to develop a synthesis method capable of precisely controlling doping, inhibiting oxidation and improving crystallization quality, so as to promote the practical application of the new generation of lead-free photoelectric nano materials. Disclosure of Invention In order to solve the problems, the invention aims to provide a convenient, efficient and low-cost microwave-assisted one-step synthesis method and application of a high-stability Cs 2ZnCl4:Cu+ nanometer luminescent material. In order to achieve the above purpose, the microwave-assisted one-step synthesis method of the high-stability Cs 2ZnCl4:Cu+ nanometer luminescent material provided by the invention comprises the following steps in sequence: 1) Weighing Cs 2H3O2、ZnCl2, cuCl and trioctylphosphine oxide serving as reaction raw materials according to a proportion, placing the mixture in a container, then adding oleic acid, oleylamine and 1-octadecene serving as surfactants according to a proportion, and uniformly stirring to prepare a mixture; 2) Placing a magnetic stirrer in a container, sealing the container, placing the container and the mixture in the container in a microwave reactor, heating the container and the mixture under stirring until the synthesis reaction is completed, and quenching the reaction by using an ice water bath; 3) And washing the reaction product with an organic solvent and dispersing the reaction product in n-hexane to obtain the high-stability Cs 2ZnCl4:Cu+ nanometer luminescent material which emits bright green light under the excitation of ultraviolet light. In the step 1), the stoichiometric ratio of the reaction raw materials is Cs +：(Zn2++Cu+) =1:2, wherein the doping concentration of Cu + is 2-30%, the stoichiometric ratio of trioctylphosphine oxide to Cs+ is (0.5-2): 2, the amount of oleic acid is 1-4 mL when each 0.2mmol of Cs+ is added, the stoichiometric ratio of oleic acid/oleylamine is (0.25-4): 1, and the amount of 1-octadecene is 1-3 mL when each 0.2mmol of Cs+ is added. In the step 1), the doping concentration of Cu +%, the stoichiometric ratio of trioctylphosphine oxide to Cs+ is 1:2, the consumption of oleic acid is 4mL when 0.2mmol of Cs+ is added, the stoichiometric ratio of oleic acid to oleylamine is 4:1, and the consumption of 1-octadecene is 2mL when 0.2mmol of Cs+ is added. In step 2), the synthesis reaction is carried out in a microwave reactor at a temperature of 60-160 ℃ for a period of 5-30 min. The temperature of the synthesis reaction is 120 ℃ and the time is 20min. In the step 3), the organic solvent is selected from ethyl acetate and n-hexane, and the washing method is that the ethyl acetate is washed three times and the n-hexane is washed once. The high-stability Cs 2ZnCl4:C