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Preparation method of copper-based perovskite nanocrystalline film

A perovskite and nanocrystalline technology, applied in the field of preparation of copper-based perovskite nanocrystalline thin films, can solve the problems of component segregation, ordinary film quality, impurity of perovskite thin films, etc. The effect of the signal-to-noise ratio

Pending Publication Date: 2021-06-25
襄阳汽车职业技术学院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventionally, the solution method is used to form the film, and the solvent will volatilize during the preparation process, which is easy to form voids and the quality of the film is ordinary; another method is the vacuum method, which is mostly concentrated in the preparation of the film. In the preparation of calcium titanium Mineral thin films often have serious component segregation problems, resulting in impure perovskite thin films. In addition, crystals cannot grow in large areas. Therefore, the vacuum method is not the preferred method for preparing perovskite thin films.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

specific Embodiment 1

[0022] The following is a specific example one based on the preparation method of the copper-based perovskite nanocrystalline thin film of the present invention: preparation of Cs 3 Cu 2 Cl 5 Nanocrystalline thin film method steps:

[0023] (1) Add 2.93g (9 mm) Cs in sequence 2 CO 3 , 0.95 ml oleic acid OA, 15 ml octadecene ODE were added to a 50 ml three-necked flask, and nitrogen gas was introduced;

[0024] (2) Heat the three-necked flask to 120°C in an oil bath and dry for 1 hour;

[0025] (3) Increase the heating temperature to 150°C, and continue to feed nitrogen until Cs 2 CO 3 , Oleic acid OA and octadecyl ODE react completely;

[0026] Note: Since cesium oleate will precipitate at room temperature, it needs to be heated to 120°C before hot injection.

[0027] (4) Weigh 0.594 g CuCl (6 mm) and 10 ml octadecene ODE, add them to another 50 ml three-necked flask, and pass nitrogen gas to remove the air in the bottle;

[0028] (5) Put the three-necked flask in ste...

specific Embodiment 2

[0038] The following is a specific example two based on the preparation method of the copper-based perovskite nanocrystalline thin film of the present invention: preparation of Cs 3 Cu 2 Br 5 Quasi-single crystal thin film method steps:

[0039] (1) Add 2.93g (9 mm) Cs in sequence 2 CO 3 , 0.95 ml oleic acid OA, 15 ml octadecene ODE were added to a 50 ml three-necked flask, and nitrogen gas was introduced;

[0040] (2) Heat the three-necked flask to 120°C in an oil bath and dry for 1 hour;

[0041] (3) Increase the heating temperature to 150°C, and continue to feed nitrogen until Cs 2 CO 3 , Oleic acid OA and octadecyl ODE react completely;

[0042] Note: Since cesium oleate will precipitate at room temperature, it needs to be heated to 120°C before hot injection.

[0043] (4) Weigh 0.861g CuBr (6 mm) and 10ml octadecene ODE, add them to another 50ml three-necked flask, and pass nitrogen gas to remove the air in the bottle;

[0044] (5) Put the three-necked flask in s...

specific Embodiment 3

[0054] The following is a specific embodiment three based on the preparation method of copper-based perovskite nanocrystalline thin film of the present invention: preparation of Cs 3 Cu 2 I 5 Method steps for nanocrystalline film:

[0055] (1) Add 2.93g (9 mm) Cs in sequence 2 CO 3 , 0.95ml oleic acid OA, 15ml octadecene ODE were added to a 50 ml three-necked flask, and nitrogen gas was passed into it;

[0056] (2) Heat the three-necked flask to 120°C in an oil bath and dry for 1 hour;

[0057] (3) Increase the heating temperature to 150°C, and continue to feed nitrogen until Cs 2 CO 3 , Oleic acid OA and octadecyl ODE react completely;

[0058] Note: Since cesium oleate will precipitate at room temperature, it needs to be heated to 120°C before hot injection.

[0059] (4) Weigh 1.143g CuI (6 mm) and 10ml octadecene ODE, add them to another 50ml three-necked flask, and pass nitrogen gas to remove the air in the bottle;

[0060] (5) Put the three-necked flask in step 4...

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Abstract

The invention discloses a preparation method of a copper-based perovskite nanocrystalline thin film, which comprises the following steps of: in the process of sintering perovskite nanocrystalline powder into a perovskite thin film, firstly, putting the dried perovskite nanocrystalline powder into a mold cavity, and pressing the dried perovskite nanocrystalline powder into a cylindrical biscuit with the diameter of phi 20mm*10mm by using a cold pressing method in a nitrogen atmosphere; inserting the pressed cylindrical blank into a Mo crucible; and then installing a multi-anvil device, and performing six-axis extrusion in the axial direction of the six tungsten carbide anvils. The ultra-high pressure can greatly reduce the sintering temperature, so that the copper-based perovskite nanocrystalline powder can form a molten state below a thermal cracking temperature point, and meanwhile, the ultra-high pressure can promote rearrangement of copper-based perovskite nanocrystals, and preferred orientation enables system free energy to move towards a lower direction, so that the copper-based perovskite thin film with the millimeter-level thickness is finally obtained.

Description

technical field [0001] The patent of the present invention relates to the technical field of perovskite film preparation, in particular to a method for preparing a copper-based perovskite nanocrystalline film. Background technique [0002] X-ray detection materials are of great significance in customs security inspection, nuclear reaction monitoring, medical imaging, etc. because of their ability to convert X-rays into electronic or optical signals. Therefore, it is particularly important to obtain X-ray detection materials with high sensitivity and high detection efficiency. In recent years, all-inorganic cesium lead halide perovskites (Cs 3 Cu 2 x 5 , X = Cl, Br, I) Quantum dots (QDs) have been widely studied due to their high luminous efficiency, simple tunable photoluminescence in the visible range, and sensitivity to X-rays. For example, in X-ray radiation detection and medical imaging, due to its excellent radioluminescent properties, it is considered to be the most...

Claims

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Application Information

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IPC IPC(8): C01G3/00B82Y40/00C09K11/61H01L31/0232
CPCC01G3/006B82Y40/00C09K11/616H01L31/02322Y02E10/549
Inventor 马安朋
Owner 襄阳汽车职业技术学院
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