A centimeter-sized graphdiyne synthesized by liquid-liquid interface polymerization and its preparation method and application

A technology of graphyne and solution, which is applied in the field of centimeter-scale graphyne and its preparation, which can solve the problems of difficult uniformity of graphyne film thickness and shape, limit the application of graphyne products, and uncontrollable synthesis, and achieve good continuous uniformity , excellent electronic properties, and structurally stable effects

Active Publication Date: 2022-05-27
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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  • A centimeter-sized graphdiyne synthesized by liquid-liquid interface polymerization and its preparation method and application
  • A centimeter-sized graphdiyne synthesized by liquid-liquid interface polymerization and its preparation method and application
  • A centimeter-sized graphdiyne synthesized by liquid-liquid interface polymerization and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1: Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as an alkynyl monomer

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

[0039] (1) Under room temperature conditions, the tetraphenylmethane and bromine element were added to the flask and stirred for 5 h, the resulting product was transferred to the environmental conditions of -78 °C, and the ethanol solution was slowly added until the precipitate was no longer generated; the precipitate product was washed and separated with sodium thiosulfate saturated solution, and the separated product was purified by the column to give the white solid product A (510mg, 29%).

[0040] (2) 0.8 g of white solid product A, 108 mg of PdCl 2 Dissolve 24.6 mg of CuI in 30 mL of i-Pr 2 NH and 0.86 mL of trimethylsilyl acetylene solution, and after reacting under nitrogen protection conditions for 42 h, the resulting product was purified by a column to give the off-white solid product B (0.6 g, 67%)...

Embodiment 2

[0057] Example 2 Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as an alkynyl monomer

[0058] To perform a reaction similar to that in Example 1, in addition to the concentration of the tetra (4-ethynylphenyl) methane solution in Example 1 becomes 1 mM, the amount of concentration ratio of the substance controlling tetra (4-ethynylphenyl) methane, copper acetate and pyridine is 10: 20: 1. By this reaction, a graphite alkyne film with transverse dimensions in the centimeter level is obtained. Compared with the graphite alkyne film obtained under the conditions of Example 1, the graphite alkyne film obtained under this condition is thinner and more fragile, relatively speaking, the graphite alkyne film structure of Example 1 is more stable.

Embodiment 3

[0059] Example 3 Preparation of graphite alkyne film with tetras (4-ethynylphenyl) methane as alkyne monomer

[0060] To perform a reaction similar to that in Example 1, in addition to the concentration of the tetra (4-ethynylphenyl) methane solution in Example 1 becomes 4 mM, the amount of concentration ratio of the material controlling tetra (4-ethynylphenyl) methane, copper acetate and pyridine is 40: 20: 1. By this reaction, a graphite alkyne film with transverse dimensions in the centimeter level is obtained. Compared with the graphite alkyne film obtained under Example 1, the graphite alkyne film obtained under this condition is thicker, but the cost is higher, and the economic applicability is not as good as In Example 1.

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PUM

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Abstract

The invention discloses a centimeter-scale graphyne synthesized by liquid-liquid interface polymerization, a preparation method and an application thereof. The preparation method of the graphyne film comprises the following steps: dissolving the alkyne-based monomer in an organic solvent to obtain an organic phase solution; dissolving copper ions and nitrogen-containing ligands in an aqueous phase solvent to obtain an aqueous phase solution; The aqueous phase solution containing copper ions and nitrogen-containing ligands is added dropwise to the upper layer of the organic phase solution to form a reaction system with a two-phase solution and then stand still to obtain a centimeter-sized graphdiyne membrane. The invention can synthesize a self-supporting large-area uniform and continuous graphyne film without substrate support, and does not need to peel the graphyne film from the substrate, avoiding the influence of the etching substrate on the performance of the graphyne product, and can directly The characterization and application of graphdiyne membrane products have broad application prospects in the fields of photoelectrochemistry, energy, catalysis, electronics, biomedicine, and materials.

Description

Technical field [0001] The present invention belongs to the field of electrochemistry, materials technology. More specifically, it involves a centimeter-sized graphyne synthesized by a liquid-liquid interface polymerization reaction and a preparation method and application thereof. Background [0002] As we all know, carbon atoms can pass through sp, sp 2 and sp 3 The three hybrid forms are bonded, and according to their different hybrid forms and rich periodic characteristics, a variety of carbon allotropes can be obtained. Traditional carbon materials include charcoal, activated carbon, natural graphite and natural diamond. New carbon materials include carbon fiber, porous carbon, glass carbon, and star carbon materials such as fullerene, carbon nanotubes, and graphene. Because of their different structures, these carbon materials exhibit very different physicochemical properties. For example, sp 3 Hybridized diamond is the hardest material in nature and is an insulator; and sp...

Claims

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Application Information

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Patent Type & Authority Patents(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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