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Ternary metal halide with ultrahigh fluorescence efficiency and preparation method

A ternary metal and halide technology, applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low luminous efficiency and difficult application in luminescent fields, and achieve good stability

Active Publication Date: 2022-02-11
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Rb 4 CdCl 6 Belongs to a ternary metal halide, where [CdCl 6 ] 4- The octahedron is surrounded by Rb + The cations are completely separated from each other, due to the completely isolated [CdCl 6 ] 4- The octahedron is inert to changes in the local crystal field environment, so the substance has good stability, but the applicant found that Rb 4 CdCl 6 The luminous efficiency is not high, it is difficult to be applied in the field of luminescence

Method used

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  • Ternary metal halide with ultrahigh fluorescence efficiency and preparation method
  • Ternary metal halide with ultrahigh fluorescence efficiency and preparation method
  • Ternary metal halide with ultrahigh fluorescence efficiency and preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Weigh 4mmol rubidium chloride, 0.9mmol anhydrous cadmium chloride, and 0.1mmol stannous chloride in the glove box, pour them into a medium mortar and grind them thoroughly, mix them evenly and transfer them to a hydrothermal reaction kettle, the above process All performed in a glove box. Next, add 4 mL of concentrated hydrochloric acid, 200 μL of hypophosphorous acid, and 0.1 mmol of sodium citrate into the reaction kettle. Seal the reaction kettle and put it into a tube furnace. Set the program to raise the temperature from room temperature to 170 ° C over 180 minutes, and maintain at this temperature 600min, then slowly cool down to room temperature at 5°C / h to obtain powdered Rb 4 CdCl 6 Crystals, the obtained crystals were transferred to a Buchner funnel covered with filter paper for suction filtration, and the crystals were continuously washed with isopropanol during the suction filtration process. Immediately afterwards, immerse the crystal in 3mL ethanol solut...

Embodiment 2

[0023] The consumption of the concentrated hydrochloric acid in the example 1 is changed to 2mL, 3mL, 5mL, 7mL respectively by 4mL, other conditions and steps are constant, Rb 4 CdCl 6 : The fluorescence efficiencies of Sn are 90.1%, 91.4%, 94.6%, and 90.8%, respectively, so 4mL of hydrochloric acid is the most optimal amount.

Embodiment 3

[0025] In Example 1, since Sn 2+ Instability, it is very easy to generate oxidation reaction to form Sn in high temperature acidic solution 4+ , has an adverse effect on the fluorescence quantum yield of the product, so hypophosphorous acid must be added. The amount of hypophosphorous acid was changed from 200 μL in Example 1 to 50 μL, 150 μL, and 300 μL respectively, and other conditions and steps remained unchanged. The measured fluorescence efficiencies of each product were 49.1%, 89.8%, and 80.3%, respectively, so the amount of hypophosphorous acid was 200 μL best.

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Abstract

The invention relates to a ternary metal halide with ultrahigh fluorescence efficiency and a preparation method thereof, and belongs to the technical field of perovskite crystal material preparation. The ternary metal halide is a Sn-doped Rb4CdCl6 perovskite fluorescent material, and is prepared by the steps of mixing rubidium chloride, anhydrous cadmium chloride and tin chloride, uniformly grinding, transferring into a hydrothermal reaction kettle, adding concentrated hydrochloric acid, hypophosphorous acid and sodium citrate, sealing the reaction kettle, putting into a tubular furnace, heating to 110-200 DEG C, maintaining for 600 minutes, slowly cooling to room temperature at the speed of 5 DEG C / h, and performing suction filtration, washing, drying, cooling treatment and the like. The Rb4CdCl6 powdery microcrystal with the ultrahigh fluorescence quantum yield close to 100% is synthesized through a simple hydrothermal method, the material emits dazzling blue-green fluorescence under excitation of an ultraviolet lamp, and the material has ultrahigh stability.

Description

technical field [0001] The invention belongs to the technical field of preparation of perovskite crystal materials, in particular to a method for significantly improving Rb by doping 4 CdCl 6 Synthetic methods for quantum efficiency. Background technique [0002] With the advancement of science and technology, people's research on fluorescence has become more and more in-depth. High-efficiency fluorescent materials have shown great application potential in the fields of white light LEDs and fluorescent probes. Existing fluorescent materials are mainly divided into rare earth fluorescent materials, metal halide fluorescent materials and organic light emitting materials. Rare earth fluorescent materials have the advantages of strong emission ability in the visible light region, but rare earth elements are irreplaceable, and the earth’s abundance is low; most metal halides have a luminous efficiency of less than 90%, and the luminous efficiency is not high; while organic fluo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/61
CPCC09K11/665
Inventor 解仁国姚佳利汪大洋杨文胜
Owner JILIN UNIV
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