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Method for accurately preparing single-layer graphdiyne or graphdiyne with certain layer number and few layers

A graphyne, single-layer technology, applied in the field of carbon material preparation, can solve the problems of inability to obtain a single-layer graphyne structure, random thickness distribution of graphyne, and difficult separation of graphyne fragment mixture

Active Publication Date: 2022-08-09
PEKING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mixture of graphyne fragments obtained based on this method is difficult to separate, and the thickness distribution of graphyne is relatively random, so it is difficult to controlly obtain separable single-layer graphyne and few-layer graphyne with a specified number of layers.
In addition, the current "bottom-up" synthesis method cannot obtain single-layer graphyne with a clear structure.
Therefore, the preparation of single-layer graphyne is still extremely challenging and has attracted much attention.

Method used

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  • Method for accurately preparing single-layer graphdiyne or graphdiyne with certain layer number and few layers
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  • Method for accurately preparing single-layer graphdiyne or graphdiyne with certain layer number and few layers

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Experimental program
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Embodiment 1

[0023] (1) Materials and methods

[0024] 1. Experimental materials

[0025] The small layer of graphite material is synthesized by the supercritical carbon dioxide reaction system (this synthesis method has been applied for patents). Depirolic uranium purchases from Beijing Shicheng Company. Iodine single purchases from Beijing Enokai Technology Co., Ltd., with a purity of 99.999%. The super -drying epoxy Sixth Ring Road was purchased at Beijing Eno Kai Technology Co., Ltd., and the oxygen content was less than 50 PPM. Tetrahydrous Fu was purchased at Beijing Enokai Technology Co., Ltd., and it was further removed by solvent purification and water oxygen removal of molecular sieves and metal sodium.

[0026] 2. Experimental instrument

[0027] Graphite's initial material synthesis experiments were performed in the supercritical fluid extract (100 ml, Separex, France). Raman spectrum uses DXRXI -type micro -Riman imaging spectrometer produced by Saimmer (USA) to detect. X-ray opto...

Embodiment 2

[0043] Change the concentration of tethalmodiaxide solution to 52 PPM. The remaining conditions are the same as the embodiment. similar. The XPS representation and embodiments in this embodiment are basically the same as the implementation example 1, the signal of the Raman spectrum ( Figure 4 ) It is basically the same as the implementation example one, but the signal intensity is higher. It should be that the specific layer number is more than the implementation example one, and the Raman spectrum is judged as four layers.

Embodiment 3

[0045] Change the concentration of tethyloxide tetrahydrous solution to 17.5 PPM, and reduce the concentration of the forefront material to 0.3 mg / ml in the graphite supercritical synthesis steps. About one -third of the thickness of the material, that is, the thickness is three layers. The remaining conditions are the same as the embodiment. The corresponding single -layer graphite material is obtained. The single -layer graphite in this embodiment is similar to the two layers of graphite in the embodiment 1. The XPS representation and embodiments 1 in this embodiment are basically the same. The signal of the Raman spectrum is basically the same as the implementation example. Figure 5 ), But compared to figure 1 The strength of the signal (A) is lower, and it should be that the specific layer number is less than the embodiment 1. Through the AFM test, it can be found that except for the height of the edge curling, the thickness of the material is about 0.4 nm, and the instrument ...

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Abstract

The invention discloses a method for accurately preparing a single layer or a certain number of layers of few-layer graphdiyne, which comprises the following steps of: performing reduction etching on the substrate-loaded few-layer graphdiyne serving as an initial material by using low-valence uranium, namely soaking the substrate-loaded few-layer graphdiyne in a low-valence uranium solution with a certain volume and concentration for a period of time under the condition of isolating water, oxygen and nitrogen; and then taking out the material, and cleaning the low-valence uranium on the material to obtain a single layer of graphdiyne or a certain number of layers of few-layer graphdiyne. According to the method, accurate preparation of single-layer graphdiyne or few-layer graphdiyne with the specified layer number is achieved by adjusting the concentration, the solution volume, the etching time, the etching temperature, the etching mode and other factors of the low-valence uranium etching solution. According to the method, the single-layer or few-layer graphdiyne with the uniform layer number is obtained through the low-valence uranium reductive etching means, generation of graphdiyne mixtures with different layer numbers is avoided, and compared with the prior art, the single-layer or few-layer graphdiyne product with the high purity can be obtained.

Description

Technical field [0001] The present invention is a carbon material preparation technology field, which specializes in a method of precisely preparing single -layer or a certain layer of graphite graphite by low -cost uranium restoration. Background technique [0002] Graphite is a carbon atom and SP hybridized by SP 2 The new type of carbon single-quality two-dimensional materials composed of hybrid carbon atoms (C.S. HUANG, Y.J. Li, N. Wang, Y.R. XUE, Z.C. Zuo, H.B. LIU, Y.L. Li. Progress Into 2D Graphdiyne-Based Matelials [J]. Chem.rev. 2018, 118, 7744-7803), the field of catalytic (R.J. LIU, H.B. LIU, Y.L.L. Li, Y.P. YI, x.k. Shen, S.S. ZHANG, X.L. YU, S.J. ZHANG, H.B. CAO, G.J. ZHANG. Nitrogen-doped graphdiyne as a metal-free catalyst for high-performance oxygenreduction reactions [J]. Nanoscale 2014, 6, 11336-11343),磁学领域(M.J. Zhang,X.X. Wang, H.J. Sun, N. Wang, Q. Lv , W.W. Cui, Y.Z. Long, C.S. Huang.Enhanced paramagnetism of mesoscopic graphdiyne by doping with nitrogen [J]....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/15
CPCC01B32/15Y02E30/30
Inventor 沈兴海熊世杰张雨晨
Owner PEKING UNIV