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CN-118325604-B - High fluorescence quantum yield Sb3+: Cs2NaInCl6Perovskite preparation method

CN118325604BCN 118325604 BCN118325604 BCN 118325604BCN-118325604-B

Abstract

The invention relates to a preparation method of high fluorescence quantum yield Sb 3+ :Cs 2 NaInCl 6 perovskite, belonging to the technical field of inorganic luminescent material preparation. Firstly, cesium chloride, sodium chloride, indium chloride and antimony chloride are mixed and ground, the obtained powder is placed in a vacuum drying oven for heat treatment at 60-300 ℃ for 0.5-2h, a mixture of oleylamine and oleic acid is added, grinding is continued until the solution becomes uniform, a hydrochloric acid solution with pH value of 3.2 is added into the product, DOPC is added into the product immediately after grinding is continued to be uniform, blue fluorescence of the product is observed to be strong, and the inorganic perovskite of Sb 3+ :Cs 3 TbCl 6 NCs with high purity and high fluorescence efficiency is obtained. The preparation of the doped Sb 3+ :Cs 2 NaInCl 6 NCs is realized through mechanical grinding for the first time, the fluorescence efficiency of the doped Sb 3+ :Cs 2 NaInCl 6 NCs is obviously enhanced through post-treatment, and the preparation method provides a good prospect for the application of Sb 3+ :Cs 2 NaInCl 6 in the aspect of photoelectricity.

Inventors

  • ZHANG ZIXU
  • YU YANG
  • GUO XIAOLIANG
  • JIN LONGYI

Assignees

  • 延边大学

Dates

Publication Date
20260512
Application Date
20240409

Claims (5)

  1. 1. A preparation method of high fluorescence quantum efficiency Sb 3+ : Cs 2 NaInCl 6 perovskite comprises the steps of firstly mixing cesium chloride, sodium chloride, indium chloride and antimony chloride according to a molar ratio of 2:1:0.9:0.1, grinding the mixture from fluffy white powder to become compact gradually and attached to agate walls, stopping grinding, radiating the mixture under an ultraviolet lamp with an excitation wavelength of 302nm, placing the obtained powder in a vacuum drying oven for heat treatment at 60-300 ℃ for 0.5-2h, adding a mixture of oleylamine and oleic acid into the mixture, wherein the volume ratio of oleylamine oleic acid is 5:1, continuously grinding until the solution becomes uniform, adding hydrochloric acid solution with a pH=3.2 into the product, continuously radiating the mixture into the product under the condition that the excitation wavelength is 5-10ml for each 1mmol of cesium chloride, and radiating the mixture into the ultraviolet lamp with a fluorescence enhancement effect of high fluorescence quantum efficiency of 3+ : Cs 2 NaInCl 6 nm, wherein the fluorescence quantum efficiency of the obtained powder is remarkably enhanced by adding DOPC (fluorescent lamp) into the ultraviolet lamp with the excitation wavelength of 5-10 ml.
  2. 2. The method for preparing a high fluorescence quantum efficiency Sb 3+ : Cs 2 NaInCl 6 perovskite according to claim 1, wherein the vacuum heat treatment is performed at 180 ◦ C for 0.5h.
  3. 3. A method of preparing a high fluorescence quantum efficiency Sb 3+ : Cs 2 NaInCl 6 perovskite according to claim 1, characterised in that 900 μl of a mixture of oleyl amine oleic acid is used per 1mmol cesium chloride.
  4. 4. The method for preparing a high fluorescence quantum efficiency Sb 3+ : Cs 2 NaInCl 6 perovskite according to claim 1, wherein the amount of the hydrochloric acid solution having ph=3.2 is 0.4ml of hydrochloric acid solution per 1mmol of cesium chloride.
  5. 5. The method for preparing high fluorescence quantum efficiency Sb 3+ : Cs 2 NaInCl 6 perovskite according to claim 1, wherein 5ml of DOPC is used for 1mmol of cesium chloride.

Description

Preparation method of high fluorescence quantum yield Sb 3+: Cs2NaInCl6 perovskite Technical Field The invention belongs to the technical field of inorganic luminescent material preparation, and particularly relates to a novel method for preparing an Sb 3+：Cs2NaInCl6 all-inorganic perovskite nano material with high fluorescence quantum efficiency. Background Lead halide perovskite has a narrow half-peak width, high fluorescence quantum efficiency and a band gap value which can be flexibly regulated and controlled, so that the lead halide perovskite is a star material in the field of photoelectric materials because of being greatly and wonderful in the fields of light emitting diodes, solar cells, photoelectric detectors, biological imaging and the like. However, the use of lead halide perovskites in the photovoltaic field is limited by the problems of poor structural stability and toxicity of the heavy metal Pb. In recent years, many scientists have attempted to replace highly toxic lead with other environmentally friendly elements of the same valence state (such as tin and germanium) while maintaining their excellent optoelectronic properties. However, the stability of Sn 2+ and Ge 2+ is also poor, which is disadvantageous for further development in the photovoltaic field. Double layer perovskite is one of the most promising candidates for non-lead perovskite because of its broad metal element selectivity and stable structure. Despite the widespread interest of double layer perovskite, its inherent structure makes its presence of transition forbidden leading to a very low fluorescence quantum efficiency (PLQY) of the material. Currently, jahn-Teller distortion of soft lattice octahedra of perovskite upon excitation by chemical doping, the generation of self-limiting domain exciton (STE) emission is one of the most effective strategies to regulate the energy band structure and fluorescence properties of double-layer perovskite. Importantly, such double layer perovskite can serve as a good host material for a variety of optical dopants. Over the last two years, various equivalent substitutions have been achieved in double layer perovskite to enhance PLQY. ,, in particular, large trivalent f-electron dopants or s-electron dopants, such as Bi 3+ or Sb 3+, in Cs 2NaInCl6 can replace the In 3+ position In the octahedral network. Sb 3+ is introduced into the B site of Cs 2NaInCl6, so that odd-even forbidden transition is broken, instability and toxicity of lead-based perovskite are solved, and fluorescence efficiency and environmental friendliness are improved. This makes it more competitive in future applications of solar cells, photodetectors, in particular lighting and displays. Therefore, the synthesis method of the Sb-doped Cs 2NaInCl6 double-layer perovskite nano material brings about wide attention to scientists, and in addition, the perovskite emits glaring blue light under ultraviolet excitation, so that the method has wide application prospect in the fields of short-cut blue photons and photoelectrons. The Zhuang group synthesized Cs 2NaInCl6 NCs using a high temperature hydrothermal method. Cs (OAc), na (OAc), in (OAc) 3 and Sb (OAc) 3 were mixed In a composition ratio of 2:1:0.45:0.05, and added to a flask together with oleylamine, oleic acid, and octadecene, and vigorously stirred under vacuum at 120 ◦ C for 30 min, then charged with N 2, kept at 120 ◦ C for 5-10 min, after white powder was dissolved, the reaction system was heated to 177 ◦ C, and finally tmcl was injected. After 30s of reaction the mixture was cooled with a water bath and PLQY was 36.9%. Cesium acetate, anhydrous sodium acetate, sb oleic acid precursor, hydrated acetic acid, oleic acid and oleic acid mixed solution are placed into a three-neck round flask according to a molar ratio of 2:1 by adopting a method of thermal injection, octadecene is added at 120 ℃ for degassing of 1h, then tri-N-octyl phosphine is injected under an N 2 atmosphere, and the obtained Sb 3+: Cs2NaInCl6 NCs PLQY reaches 39.1%. Although the synthetic method can synthesize Sb 3+: Cs2NaInCl6 NCs, the operation is complex, the participation of an organic solvent is needed, the time consumption is long, the long-time heating reaction at a higher temperature is needed, the energy consumption is high, the large-scale production is not facilitated, and the application of the method in the photoelectric field is limited. The synthesis method is subject to further improvement and innovation. Therefore, the novel method for preparing the Sb 3+: Cs2NaInCl6 NCs, which is environment-friendly, pollution-free, and capable of efficiently synthesizing and improving the fluorescence quantum efficiency, has very important significance for the large-scale production and application of the inorganic perovskite nano material. Disclosure of Invention The technical problem to be solved by the invention is to overcome the problems existing in the background technology, and provide