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Preparation method and application of adjustable porphyrin MOFs film

A technology of porphyrin and thin film, which is applied in the field of preparation of adjustable porphyrin MOFs thin film, which can solve the problems of poor binding ability between MOFs and the substrate, difficulty in meeting the application requirements of large area and thin film of the detector, and difficulty in direct film formation, etc. , to achieve the effect of short time, simple operation and large degree of electron delocalization

Active Publication Date: 2022-07-26
MINJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, MOFs materials mostly exist in the form of powder / bulk, and the bonding ability of powder MOFs to the substrate is poor, so it is difficult to directly form a film, and it is difficult to meet the application requirements of large-area and thin-film detectors.

Method used

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  • Preparation method and application of adjustable porphyrin MOFs film
  • Preparation method and application of adjustable porphyrin MOFs film
  • Preparation method and application of adjustable porphyrin MOFs film

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] The preparation of metallated porphyrin ligands (TCPP(M), M=Zn, Mn, Fe) includes the following steps:

[0045] (1) Preparation of TPPCOOMe

[0046] Pyrrole (6.0 g, 0.086 mol) and methyl p-formylbenzoate (12 g, 0.086 mol) were heated to reflux in 100 mL propionic acid for 12 h. After the reaction mixture was cooled to room temperature, the solid was collected under reduced pressure and dried.

[0047] (2) Preparation of TPPCOOMe (M)

[0048] Take TPPCOOMe(Mn) as an example: combine TPPCOOMe (0.854g, 1.0mmol) with MnCl 2 ·6H 2 A solution of O (3.1 g, 12.8 mmol) was heated to reflux in 100 mL of DMF for 8 h, cooled to room temperature and then added with 150 mL of water. The resulting precipitate was used 50mlH 2 O filter wash twice. The resulting solid was dissolved in CHCl 3 , washed three times with water, and dried to obtain a certain amount of dark red powder.

[0049] The synthetic routes of TPPCOOMe(Zn) and TPPCOOMe(Fe) are the same as those of TPPCOOMe(Mn) ...

Embodiment 2

[0054] (1) 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin zinc (TCPP(Zn)) ligand was first prepared by the method of Example 1.

[0055] (2) Preparation of hydroxyl-functionalized growth substrates

[0056] A mixed solution of 98% sulfuric acid and 30% hydrogen peroxide (3:1 by volume) was prepared for later use, and then the oil and impurities on the surface of the silica / silicon substrate were cleaned with organic solvent and distilled water in turn. Immerse the silica / silicon substrate in the above mixed solution, heat it in a water bath at 80°C for 40 min, pour out the mixed solution after the reaction, rinse the silica / silicon substrate several times with clean water, and wash the surface of the mixture The solution was rinsed with ethanol, and finally dried with nitrogen to obtain a hydroxyl-functionalized silica / silicon substrate. Among them, concentrated sulfuric acid can also be replaced by sodium hydroxide aqueous solution.

[0057] (3) Preparation of ZnTCPP(Zn) thi...

Embodiment 3

[0064] (1) 5,10,15,20-tetrakis(4-carboxyphenyl)porphyrin manganese (TCPP(Mn)) ligand was first prepared by the method of Example 1.

[0065] (2) Preparation of functionalized growth substrates

[0066] A mixed solution of 98% sulfuric acid and 30% hydrogen peroxide (3:1 by volume) was prepared for later use, and then the oil and impurities on the surface of the silica / silicon substrate were cleaned with organic solvent and distilled water in turn. Immerse the silica / silicon substrate in the above mixed solution, heat it in a water bath at 80°C for 40 min, pour out the mixed solution after the reaction, rinse the silica / silicon substrate several times with clean water, and wash the surface of the mixture solution, rinsed with ethanol, and finally dried with nitrogen to obtain hydroxyl-functionalized silica / silicon substrates. Concentrated sulfuric acid can also be replaced with aqueous sodium hydroxide solution. The hydroxyl-functionalized silica / silicon substrate can be furt...

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Abstract

The invention discloses a preparation method and application of an adjustable porphyrin MOFs film. The preparation method comprises the following steps: preparing a metallized porphyrin ligand; the method comprises the following steps: performing functional modification on a growth substrate, alternately depositing droplets of a metal salt solution and a metallized porphyrin ligand solution on the surface of the growth substrate, and growing on the surface of the growth substrate through coordination to form the porphyrin MOFs film. According to the method, the thickness, the area and the roughness of the MOFs film can be accurately controlled in the preparation process, the preparation efficiency is high, and the operation is simple. The porphyrin MOFs thin film can be used as a photoelectric conversion layer in the preparation of an optical detector, the performance of the optical detector is regulated and controlled by changing the type of central metal of a porphyrin ligand, and the prepared porphyrin MOFs-based optical detector integrates the dual advantages of metalloporphyrin and MOFs structures; and a wide prospect is provided for the application of the material in the fields of optical detectors and other devices.

Description

technical field [0001] The invention belongs to the field of device preparation, and in particular relates to a preparation method and application of a controllable porphyrin MOFs thin film. Background technique [0002] Metal-organic frameworks (MOFs), as a kind of inorganic-organic hybrid materials, are a kind of optoelectronics with great potential and development value due to their rich composition, highly ordered crystal structure, and complex and ingenious electronic arrangement. conversion layer material. However, MOFs materials mostly exist in the form of powder / bulk, and the powder MOFs have poor bonding ability with the substrate, making it difficult to directly form a film, and it is difficult to meet the application requirements of large-area and thin-film detectors. Therefore, there is an urgent need for a high-quality method for preparing MOFs thin films, which can be applied to the preparation of photoelectric conversion layers of photodetectors, and can effe...

Claims

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Application Information

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IPC IPC(8): C08L87/00C08J5/18H01L51/42H01L51/46
CPCC08J5/18C08J2387/00H10K30/30Y02E10/549
Inventor 李德晶蒲德福梁茜林棋
Owner MINJIANG UNIV
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