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High-fluorescence-efficiency inorganic lead-free perovskite material and preparation method thereof

An inorganic non-perovskite technology, applied in the direction of luminescent materials, chemical instruments and methods, can solve the problems of high energy consumption, long time consumption, and lack of fluorescent properties

Active Publication Date: 2021-03-12
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this double-layer perovskite will lead to an increase in the non-radiative recombination pathways of electrons and holes, which will reduce the fluorescence efficiency.
[0004] In 1949, the Clarabrink group prepared Cs for the first time. 2 AgI 3 This substance, due to the poor solubility of silver iodide, the synthesis needs to introduce potassium iodide under high temperature conditions, and prepare it into a concentrated solution to promote the dissolution of raw materials. This method cannot avoid the impact of excess KI on crystal purity.
In 2004, S. Hull's group also synthesized Cs by solid phase high temperature melting method. 2 AgI 3 , the method is complicated to operate, consumes a lot of energy, takes a long time, and is not conducive to large-scale industrial production
In 2020, Xie's group prepared lead-free and cadmium-free bimetallic Cs-Ag-X (X=Cl, Br, I) halides for the first time by ball milling, realizing a spectrum ranging from ultraviolet-visible to near-infrared (390 to 820nm) Wide range of tuning, the study found that in order to prepare bright yellow fluorescent Cs 2 AgI 3 A certain amount of silver acetate must be added as a photoinitiator, and Cs with fluorescent properties cannot be obtained simply by ball milling cesium iodide and silver iodide. 2 AgI 3

Method used

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  • High-fluorescence-efficiency inorganic lead-free perovskite material and preparation method thereof
  • High-fluorescence-efficiency inorganic lead-free perovskite material and preparation method thereof
  • High-fluorescence-efficiency inorganic lead-free perovskite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0023] Weigh 2mmol cesium iodide and 1mmol silver iodide in the glove box, pour them into a 25mL agate jar containing 25 agate balls with a diameter of 6mm, seal the agate jar with a sealing film, take it out of the glove box, set The AC frequency of the ball mill is 35Hz, and the corresponding rotating speed is 1050rad / min at this time. After mechanical grinding for 10 hours, the yellow-green mixture powder changes from fluffy to dense with the prolongation of the grinding time, and finally turns into a fluffy light yellow powder. Stop grinding. When irradiated with an ultraviolet lamp with an excitation wavelength of 302nm, the product has no fluorescence. Put the obtained product into a hydrothermal reaction kettle, add 0.2mol cuprous iodide, 30 microliters of hypophosphorous acid, and 2 milliliters of hydroiodic acid, maintain at 180°C for 5 hours, and cool down to room temperature through a 24h program. After annealing at room temperature, after cooling at -15 °C for 1.5 ...

Embodiment 2

[0026] In Example 1, due to Cu + Instability, it is very prone to disproportionation reaction to generate Cu 2+ and Cu, therefore hypophosphorous acid must be added, now the amount of hypophosphorous acid is changed from 30uL in Example 1 to 10uL, 20uL, 50uL respectively, other conditions and steps are unchanged, the fluorescence efficiency of each product is measured to be 59.4%, 62.8% respectively. %, 63.7%, so the optimal dosage of hypophosphorous acid is 30uL.

Embodiment 3

[0028] Change the hydroiodic acid consumption in embodiment 1 into 1mL, 1.5mL, 3mL respectively by 2mL, other conditions and steps are constant, record the fluorescence efficiency of each product to be respectively 50.4%, 54.6%, 47.1%, therefore hydroiodide The optimal acid volume is 2mL.

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Abstract

The invention discloses a high-fluorescence-efficiency inorganic lead-free perovskite material and a preparation method thereof, and belongs to the technical field of perovskite crystal material preparation. The high-fluorescence-efficiency inorganic lead-free perovskite material is Cu-doped Cs2AgI3 perovskite, and the doping amount of Cu is 0.09%. The preparation method comprises the following steps: mixing cesium iodide and silver iodide, carrying out ball milling, adding cuprous iodide, hydroiodic acid and microliter hypophosphorous acid, carrying out sealed heating to 150-200 DEG C, cooling to room temperature, annealing, and carrying out cooling treatment at -10 to -35 DEG C for 1-3 hours. The Cs2AgI3: Cu crystal with high purity and enhanced fluorescence efficiency is obtained, emitsbright blue fluorescence under the excitation of a 302 nm ultraviolet lamp, and has the advantages of no lead or chromium, high quantum efficiency, environmental stability and the like.

Description

technical field [0001] The invention belongs to the technical field of preparation of perovskite crystal materials, in particular to a method for significantly increasing Cs by doping Cu 2 AgI 3 Quantum efficiency, synthetic Cs 2 AgI 3 : Cu blue fluorescent material method. Background technique [0002] Renewable energy includes solar energy, water energy, wind energy, biomass energy, wave energy, tidal energy, ocean temperature difference energy, geothermal energy, etc. These energy sources are recyclable and renewable in nature, and are inexhaustible. If these energies can be utilized, it will greatly promote the development of human society. Therefore, photovoltaic cells that directly convert sunlight into electricity are of considerable interest. By the end of 2012, the cumulative installation of photovoltaics in the world reached about 100GWp (gigawatts). Among the solar cells in the world, 85% are crystalline silicon solar cells, and the rest are polycrystalline...

Claims

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Application Information

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IPC IPC(8): C09K11/61
CPCC09K11/616
Inventor 解仁国姚佳利张资序
Owner JILIN UNIV
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