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Method for preparing graphite alkyne film

A graphdiyne and thin film technology is applied in the field of preparing graphdiyne thin films to achieve the effects of simple process and uniform surface

Active Publication Date: 2010-07-14
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since graphyne was proposed, researchers have done a lot of research on the synthesis of its monomers and oligomers (Q.Zhou, P.J.Carroll and T.M.Swager, J.Org.Chem., 1994, 59, 1294-1301. M.M.Haley, M.L.Bell, J.J.English, C.A.Johnson and T.J.R.Weakley, J.Am.Chem.Soc., 1997, 119, 2956-2957.W.B.Wan and M.M.Haley, J.Org.Chem., 2001, 66, 3893 -3901.W.B.Wan, S.C.Brand, J.J.Pak and M.M.Haley, Chem.Eur.J., 2000, 6, 2044-2052.A.Marsden and M.M.Haley, J.Org.Chem., 2005, 70, 10213- 10226.), and this new type of carbon allotrope graphyne has not yet been synthesized

Method used

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  • Method for preparing graphite alkyne film
  • Method for preparing graphite alkyne film
  • Method for preparing graphite alkyne film

Examples

Experimental program
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Effect test

Embodiment 1

[0028] At 8°C, 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mol / L (M) tetrahydrofuran solution, 0.4 mmol), stirred and reacted for 10 minutes under nitrogen protection. Afterwards, the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to give hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, and slowly add it dropwise to a three-neck flask filled with 50ml of pyridine (pyridine) and copper foil (copper foil, 4 square centimeters) under nitrogen protection (the temperature of the reaction solution is 60°C), and the time for adding for 24 hours. The stirring reaction was then continued at 60°C for 3 days. After the reaction finishes, a black film is formed on the copper sheet, and the copper sheet is washed with acetone and N,N-dimethylformamide (DMF) successively. This black film is a graphyne film (2.7mg, 24.3%). T...

Embodiment 2

[0038] At 8°C, 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mol / L (M) tetrahydrofuran solution, 0.4 mmol), stirred and reacted for 10 minutes under nitrogen protection. Afterwards, the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to give hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, and slowly add it dropwise to a three-neck flask containing 50ml of pyridine and copper foil (4 square centimeters) under nitrogen protection (the temperature of the reaction solution is 50°C), and the time for adding for 24 hours. The stirring reaction was then continued at 50°C for 3 days. After the reaction finishes, a black film is formed on the copper sheet, and the copper sheet is washed with acetone and N,N-dimethylformamide (DMF) successively. This black film is graphyne thin film (1.3mg, 11.7%). Under this condition, t...

Embodiment 3

[0040] At 8°C, 0.4 ml of tetrabutylammonium fluoride (TBAF) (1 mol / L (M) tetrahydrofuran solution, 0.4 mmol), stirred and reacted for 10 minutes under nitrogen protection. Afterwards, the reaction solution was diluted with ethyl acetate (20 mL), washed three times with saturated brine, dried over anhydrous sodium sulfate (10 g), and concentrated to dryness to give hexaynylbenzene (compound 2) (9.08 mg, 62%). Dissolve compound 2 with 25ml of pyridine, and slowly add it dropwise to a three-neck flask filled with 50ml of pyridine (pyridine) and copper foil (copper foil, 4 square centimeters) under nitrogen protection (the temperature of the reaction solution is 80°C), and the time for adding for 24 hours. The stirring reaction was then continued at 80°C for 3 days. After the reaction finishes, a black film is formed on the copper sheet, and the copper sheet is washed with acetone and N, N-dimethylformamide (DMF) successively. This black film is graphyne thin film (2.0mg, 18.2%)...

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Abstract

The invention discloses a method for preparing a graphite alkyne film. The method comprises that: a copper sheet or any one substrate the surface of which is covered with a copper film layer is used as a substrate; 6-alkynyl-benzene is subjected to coupling reaction in a solvent under the catalytic action of the copper to obtain the graphite alkyne film on the surface of the substrate. The method for preparing the graphite alkyne film, which is provided by the invention, has simple and convenient process, and can carry out large-scale preparation of the graphite alkyne film on the surface of the copper sheet or the substrate any surface of which is covered with the copper. The electrical conductivity of the graphite alkyne film is 2.516*10-4S / m. The film has uniform surface, can exist stably in the air, is a semiconductor with similar performances with silicon, and has potential application prospect in the fields of catalysis, electron, semiconductor, energy, material and the like.

Description

technical field [0001] The invention relates to the field of semiconductors, in particular to a method for preparing a graphyne film. Background technique [0002] Graphite and diamond are two allotropes of carbon that have been known for nearly a thousand years and are widely used in real life today. In 1990, Huffman discovered the existence of fullerene (C60) (W. D.R.Huffman.Nature, 1990,347,354-358.), in 2004 Andre K.Geim et al prepared graphene for the first time (K.S.Novoselov, A.K.Geim, S.V.Morozov, D.Jiang, Y.Zhang, S.V.Dubonos, I.V. Grigorieva, A.A.Firsov.Science, 2004, 306, 666-669.), let people have a deeper understanding of carbon allotropes, and at the same time stimulated researchers to study new carbon allotropes research interests. With the rapid development of synthetic chemistry, scientists have proposed many new carbon-rich molecules, trying to synthesize new carbon allotropes, among which graphdiyne (Graphdiyne) ( figure 1 ) has a novel structure, and...

Claims

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Application Information

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IPC IPC(8): C01B31/02
Inventor 李玉良刘辉彪李国兴
Owner INST OF CHEM CHINESE ACAD OF SCI
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