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Method for preparing aza graphene and nanometer metal graphene through solid phase cracking method

A metal graphite, graphene technology, applied in the direction of graphene, nanotechnology for materials and surface science, nanocarbon, etc., can solve the problems of high cost, easy aggregation of nanoparticles, low efficiency, etc., to improve the electrical conductivity. Effect

Active Publication Date: 2014-03-26
SICHUAN HUANTAN TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, graphene nitrogen doping methods mainly include hydrothermal synthesis method, chemical synthesis method, CVD method, plasma sputtering, etc. (such as invention patents CN102887498, CN102745678, CN101708837, etc.), and the synthesis efficiency and quality of these methods are generally low
Incorporating metal nanoparticles into graphene is a common practice for electrochemical device modification and electrode modification. At present, the main composite methods include redox method, electrochemical reduction method, etc. (such as CN102174702A, CN102136306A, etc.), and the main methods of these methods are The problem is that there is a large amount of chemical waste liquid, and the nanoparticles are easy to aggregate
[0006] Therefore, there is an urgent need to develop a method that uses new raw materials, is simple and easy to implement, has no special requirements for equipment, has low cost, high efficiency, zero pollution, zero emissions, is easy to promote and use, and can solve the problems existing in the existing graphene preparation technology. High cost, low efficiency, poor quality, etc., and the method of producing azagraphene and nano-metal graphene from raw materials at one time without the need to generate intermediate product graphene

Method used

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  • Method for preparing aza graphene and nanometer metal graphene through solid phase cracking method
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  • Method for preparing aza graphene and nanometer metal graphene through solid phase cracking method

Examples

Experimental program
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Effect test

Embodiment 1

[0050] 30.0 g of commercially available copper phthalocyanine was used as the starting material without any purification treatment. In a quartz tube furnace, under the protection of high-purity argon, the flow rate of argon is controlled at 50cm 3 min -1 , 20.7 grams of final metallic graphene-like materials were obtained by cracking under the following heating scheme. That is, the temperature is raised to 300 degrees at a slow heating rate of 5 degrees per minute, and 300 degrees is stable for 1 hour; the temperature is raised to 350 degrees at 5 degrees per minute, and 350 degrees is stable for 1 hour; hour; the temperature is raised to 500 degrees at 3 degrees per minute, and 500 degrees is stable for 4 hours; the temperature is raised to 800 degrees at 2 degrees per minute, and 800 degrees is stable for 8 hours, and finally it is naturally lowered to room temperature, and graphene containing metallic copper nanoparticles is obtained. Its XRD and transmission electron mic...

Embodiment 2

[0052] Taking self-made copper phthalocyanine as a starting material, first prepare graphene containing metallic copper nanoparticles as in Example 1, and then use pure HCl, pure H 2 SO 4 Wait for the strong acid to dissolve, and after stirring at room temperature for several hours, a graphene material without metal particles is obtained. The XRD and transmission electron microscope see Figure 5 and Figure 6 .

Embodiment 3

[0054] Commercially available copper phthalocyanine is used as the starting material without any purification treatment. In a quartz tube furnace, copper foil or nickel foil is used as the base material. Under the protection of high-purity argon, the argon flow rate is controlled at 30cm 3 min -1 , the heating program is: at a slow heating rate of 5 degrees per minute to 300 degrees, 300 degrees stable for 1 hour; at 5 degrees per minute to 350 degrees, 350 degrees stable for 1 hour; at 5 degrees per minute to 400 degrees , 400 degrees stable for 1 hour; 3 degrees per minute to 700 degrees, 700 degrees for 4 hours; 2 degrees per minute to 1000 degrees, 1000 degrees for 8 hours, and finally naturally cooled to room temperature, treated with acid to obtain The graphene material doped with nitrogen atoms with a coiled structure, its topography is shown in Figure 7 .

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Abstract

The invention relates to a method for preparing aza graphene and nanometer metal graphene by using a solid phase cracking technology, wherein a phthalocyanine compound, a phthalocyanine polymer and a derivative thereof are adopted as starting raw materials, and cracking is performed at a temperature of more than 700 DEG C under an atmosphere of high purity nitrogen gas, argon gas or argon / hydrogen mixed gas to obtain the nitrogen-containing graphene and nanometer metal graphene materials. The method is characterized in that 1, the method is simple, and the aza graphene and nanometer metal graphene materials can be obtained through one-time solid phase cracking; 2, the graphene materials can be obtained through cracking in a non-hydrogen environment; 3, with adjustment on the cracking temperature, the gas flow rate and other experiment parameters, the size, the thickness and the quality of the graphene materials can be effectively controlled; and 4, the graphene materials with the coil behavior can be obtained under the catalyst effect. The prepared graphene materials can be applied in the fields of single molecule detection technologies, field-effect transistors and integrated circuits thereof, transparent conductive electrodes, conductive inks, field emission sources and vacuum electron devices thereof, supercapacitors, biological devices and the like.

Description

technical field [0001] The invention adopts a solid-phase cracking technology to prepare azagraphene and nano-metal graphene materials, and belongs to the field of high-tech material preparation. Background technique [0002] In 2004, Geim et al. used adhesive tape to repeatedly peel off graphene on natural graphite[1]. Graphene has caused an unprecedented sensation in the scientific community because of its unique single-layer flake hexagonal honeycomb lattice structure. Its unique excellent performance and The huge potential application value has attracted widespread attention all over the world. In terms of chemical bonding, the carbon atoms constituting the two-dimensional structure of graphene are represented by sp 2 This method of hybridization allows carbon atoms to form stable C-C bonds with three adjacent carbon atoms through σ bonds, endowing graphene with extremely high mechanical properties [2]. At the same time, the π electrons provided by a large number of ca...

Claims

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Application Information

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IPC IPC(8): C01B31/04B82Y30/00
CPCC01B32/184B82Y30/00B82Y40/00
Inventor 薛卫东赵睿
Owner SICHUAN HUANTAN TECH
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