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Centimeter sized graphdiyne synthesized through liquid-liquid interface polymerization reaction and application

A technology of graphyne and solution, which is applied in the field of centimeter-scale graphyne and its preparation, can solve the problems of difficulty in uniform thickness and shape of graphyne film, limit the application of graphyne products, and uncontrollable synthesis, etc., achieving good application prospects, The effect of good continuous uniformity and excellent electronic performance

Active Publication Date: 2019-04-16
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, the method of using the solid-liquid interface to synthesize graphyne film has certain limitations, and the product needs to be peeled off from the substrate. The peeling process will have a great impact on the performance of graphyne. The thickness of the graphyne film obtained by the peeling method and morphology are difficult to be uniform, and the few-layer film yield is very low
In 2017, Professor Nishihara's research group synthesized a graphyne membrane with the monomer molecule hexaethynylbenzene by means of liquid-liquid interface polymerization reaction. Limit the application of graphyne products
[0005] Therefore, the current synthesis of graphyne is still facing a huge challenge: it is still impossible to control the synthesis of a large-area uniform and continuous graphyne film that does not require inert gas protection, and the product does not need to be peeled off from the substrate.

Method used

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  • Centimeter sized graphdiyne synthesized through liquid-liquid interface polymerization reaction and application
  • Centimeter sized graphdiyne synthesized through liquid-liquid interface polymerization reaction and application
  • Centimeter sized graphdiyne synthesized through liquid-liquid interface polymerization reaction and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Preparation of graphyne membrane using tetrakis(4-ethynylphenyl)methane as alkyne monomer

[0038] 1. Preparation of tetrakis(4-ethynylphenyl)methane

[0039] (1) At room temperature, add tetraphenylmethane and bromine into the flask and stir for 5 hours, then transfer the obtained product to -78°C, and slowly add ethanol solution until no precipitation occurs; The precipitated product was washed and separated with a saturated sodium thiosulfate solution, and the separated product was purified through a column to obtain product A (510 mg, 29%) as a white solid.

[0040] (2) 0.8 g of white solid product A, 108 mg of PdCl 2 and 24.6 mg of CuI were dissolved in 30 mL of i-Pr 2NH and 0.86 mL of trimethylsilylacetylene solution, and reacted for 42 h under nitrogen protection, the obtained product was purified by column to obtain off-white solid product B (0.6 g, 67%).

[0041] (3) At room temperature, 0.6 g of product B, 0.33 g of NaOH, 10 mL of methanol and 40 ...

Embodiment 2

[0057] Example 2 Preparation of graphyne membrane using tetrakis(4-ethynylphenyl)methane as alkyne monomer

[0058] A reaction similar to that in Example 1 was carried out, except that the concentration of the tetrakis(4-ethynylphenyl)methane solution in Example 1 was changed to 1 mM, and the tetrakis(4-ethynylphenyl)methane, copper acetate The concentration ratio of the substance and pyridine is 10:20:1. Through this reaction, graphyne membranes with lateral dimensions on the order of centimeters were obtained. Compared with the graphyne film obtained under the conditions of Example 1, the graphyne film obtained under this condition is thinner and more fragile, and relatively speaking, the graphyne film structure of Example 1 is more stable.

Embodiment 3

[0059] Example 3 Preparation of graphyne membrane using tetrakis(4-ethynylphenyl)methane as alkyne-based monomer

[0060] A reaction similar to that in Example 1 was carried out, except that the concentration of the tetrakis(4-ethynylphenyl)methane solution in Example 1 was changed to 4 mM, and the tetrakis(4-ethynylphenyl)methane, copper acetate The concentration ratio of the substance and pyridine is 40:20:1. Through this reaction, graphyne membranes with lateral dimensions on the order of centimeters were obtained. Compared with the graphyne film obtained under the conditions of Example 1, the graphyne film obtained under this condition is thicker, but the cost is higher, and the economic applicability is not as good as that of Example 1.

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Abstract

The invention discloses centimeter sized graphdiyne synthesized through a liquid-liquid interface polymerization reaction and a preparation method and application thereof. The preparation method of agraphdiyne membrane comprises the following steps that an alkynyl monomer is dissolved into an organic solvent, and an organic phase solution is obtained; copper ions and a nitrogen-containing ligandare dissolved into an aqueous phase, and an aqueous solution is obtained; the aqueous solution containing copper ions and the nitrogen-containing ligand is dropped into an upper layer of the organic phase solution, a reaction system with two-phase solutions is formed, and then standing is performed, so that the centimeter sized graphdiyne membrane is obtained. The self-supporting large-area uniform-connected graphdiyne membrane can be synthesized, no substrate supporting is needed, graphdiyne does not need to be peeled from the substrate, the influence of an etching substrate on the graphdiyneproduct performance is avoided, the graphdiyne membrane product can be directly subjected to representation and application, and the application prospect in the fields of photoelectric chemistry, energy, catalysis, electronics, biological medicine and materials is wide.

Description

technical field [0001] The invention belongs to the field of electrochemistry and material technology. More specifically, it relates to a centimeter-scale graphyne synthesized by liquid-liquid interface polymerization and its preparation method and application. Background technique [0002] As we all know, carbon atoms can pass through sp, sp 2 and sp 3 The three hybridization forms form bonds, and various carbon allotropes can be obtained according to their different hybridization forms and rich periodic characteristics. Traditional carbon materials include charcoal, activated carbon, natural graphite, and natural diamond. New carbon materials include carbon fibers, porous carbon, glassy carbon, and star carbon materials such as fullerenes, carbon nanotubes, and graphene. Because of the different structures, these carbon materials exhibit very different physical and chemical properties. For example, sp 3 Hybrid diamond is the hardest material in nature and is an insul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/05
CPCC01B32/05
Inventor 郑治坤叶晓军刘卫郑治雪李忠亮
Owner SUN YAT SEN UNIV
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