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A kind of preparation method of perylenetetracarboxylic acid-graphene heterojunction based photoanode material

A technology of perylene tetracarboxylic acid and graphene, which is applied in the field of preparation of perylene tetracarboxylic acid-graphene heterojunction-based photoanode materials, and can solve unfavorable probe molecules, covalent bonding, unfavorable photoelectrochemical sensors, etc. problem, to achieve the effect of improving comprehensive analysis performance and good optical stability

Inactive Publication Date: 2015-09-09
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, most of the heterojunction semiconductors reported so far do not have active groups such as amino, carboxyl, or hydroxyl groups, so they are not conducive to covalent bonding with probe molecules, so they are not conducive to the construction of stable photoelectrochemical sensors.
The reason is that the synthesis method of the above-mentioned semiconductors, especially inorganic nano-semiconductors, determines that it is difficult to synthesize them in one step with active groups.

Method used

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  • A kind of preparation method of perylenetetracarboxylic acid-graphene heterojunction based photoanode material
  • A kind of preparation method of perylenetetracarboxylic acid-graphene heterojunction based photoanode material
  • A kind of preparation method of perylenetetracarboxylic acid-graphene heterojunction based photoanode material

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Effect test

Embodiment 1

[0016] Example 1: The preparation method of the perylene tetracarboxylic acid-graphene heterojunction-based photoanode material: firstly, the perylene tetracarboxylic acid is synthesized, and then compounded with graphene in a certain proportion. The synthesis process of perylene tetracarboxylic acid is as follows: first, add perylene tetracarboxylic dianhydride into 4% potassium hydroxide solution, and stir at 60°C until it is completely dissolved. Add 0.08 mol L dropwise with stirring -1 Hydrochloric acid solution until pH = 4.5 is obtained, wherein as the pH of the solution decreases, the formation of solid perylenetetracarboxylic acid is accompanied. After it was completely precipitated, it was filtered, washed, and vacuum-dried to obtain red perylene tetracarboxylic acid with a yield of 92.5%.

[0017] The specific scheme for preparing perylenetetracarboxylic acid / graphene heterojunction is as follows: First, prepare 0.05×10 -4 mol L -1 DMF solution of perylenetetra...

Embodiment 2

[0020] Example 2: The preparation method of perylene tetracarboxylic acid-graphene heterojunction-based photoanode material: firstly, perylene tetracarboxylic acid is synthesized, and then it is combined with graphene in a certain ratio. The synthesis process of perylene tetracarboxylic acid is as follows: first, add perylene tetracarboxylic dianhydride into 5% potassium hydroxide solution, and stir at 65°C until it is completely dissolved. Add 0.1 mol L dropwise with stirring -1 Hydrochloric acid solution until pH = 4.8 is obtained, wherein as the pH of the solution decreases, the formation of solid perylenetetracarboxylic acid is accompanied. After it was completely precipitated, it was filtered, washed, and vacuum-dried to obtain red perylene tetracarboxylic acid with a yield of 96.5%.

[0021] The specific scheme for preparing perylenetetracarboxylic acid / graphene heterojunction is as follows: First, prepare 1×10 -4 mol L -1 DMF solution of perylenetetracarboxylic ac...

Embodiment 3

[0023] Example 3:The preparation method of perylene tetracarboxylic acid-graphene heterojunction-based photoanode material: firstly, perylene tetracarboxylic acid is synthesized, and then it is combined with graphene in a certain ratio. The synthesis process of perylene tetracarboxylic acid is as follows: first, add perylene tetracarboxylic dianhydride into 6% potassium hydroxide solution, and stir at 70°C until it is completely dissolved. Add 0.12 mol L dropwise with stirring -1 Hydrochloric acid solution until pH = 5.1 is obtained, wherein as the pH of the solution decreases, the formation of solid perylenetetracarboxylic acid is accompanied. After it was completely precipitated, it was filtered, washed, and vacuum-dried to obtain red perylene tetracarboxylic acid with a yield of 97.5%.

[0024] The specific scheme for preparing perylenetetracarboxylic acid / graphene heterojunction is as follows: First, prepare 2×10 -4 mol L -1 DMF solution of perylenetetracarboxylic ac...

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Abstract

The invention discloses a preparation method of a perylene tetracarboxylic acid-graphene heterojunction based photo-anode material. The preparation method comprises the steps of (1) mixing a perylene tetracarboxylic acid DMF solution with a concentration of 0.5*10<-4>-2*10<-4> mol.L<-1> and a graphene suspension liquid with a concentration of 0.5*10<-2>-2*10<-2> mg.mL<-1> according to a proportion of 2 : 1-8 : 1 at a room temperature for 1-4 hours under the assist of ultrasonic waves, then stirring for 1-4 hours, standing for a night to produce perylene tetracarboxylic acid / graphene heterojunctions; and (2) drop casting a perylene tetracarboxylic acid / graphene heterojunction suspension liquid on the surface of a polished glassy carbon electrode and drying at a room temperature to obtain the perylene tetracarboxylic acid-graphene heterojunction based photo-anode material. The perylene tetracarboxylic acid-graphene heterojunction based photo-anode material prepared by the preparation method is a heterojunction semiconductor with active groups and can stably combine with a probe molecule, so that comprehensive analysis performance of a photoelectrochemical sensor can be improved.

Description

technical field [0001] The invention relates to a preparation method of a perylene tetracarboxylic acid-graphene heterojunction-based photoanode material. Background technique [0002] In the field of photoelectrochemical sensing, most of the research work on photoelectrochemical sensing is based on the quantitative influence of the analyte on the formation of photoelectric signals. Organic semiconductors with easy synthesis and large-area flexible fabrication such as porphyrin, ruthenium pyridine, conductive polymers, etc., and inorganic nano-semiconductors with faster carrier mobility such as SnO 2 、TiO 2 、WO 3 , BiOI, CdS, CdSe, and CdTe have been widely used in photoelectrochemical sensing platforms. Compared with single semiconductors, heterojunction semiconductors can more effectively promote the separation of electron-hole pairs, thereby improving detection sensitivity. However, most of the heterojunction semiconductors reported so far do not have active groups su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N27/30
Inventor 李红波李静王伟高雷李威
Owner YANCHENG INST OF TECH
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