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High-temperature and high-pressure preparation method of carbon nano onions

A high temperature and high pressure, high temperature and high pressure synthesis technology, applied in the application of ultra-high pressure process and other directions, can solve the problems of poor controllability, low purity and high energy consumption, and achieve the effect of improving performance, high purity and low energy consumption

Inactive Publication Date: 2016-08-10
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these methods all have one or several disadvantages of high energy consumption, low yield, low purity and poor controllability.

Method used

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  • High-temperature and high-pressure preparation method of carbon nano onions
  • High-temperature and high-pressure preparation method of carbon nano onions
  • High-temperature and high-pressure preparation method of carbon nano onions

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The nano-diamond powder with an average particle size of 9nm is pressed into shape by a hydraulic press, and then the sample is loaded into the synthesis chamber. Graphite tubes are used to heat the assembly chamber, pyrophyllite is used as insulation material, and hexagonal boron nitride is used to protect the chamber. The synthesis pressure is 1.0GPa, the synthesis temperature is 1273K, and the heat preservation and pressure holding time is 15 minutes. After the heating is stopped, the sample is naturally cooled to After releasing the pressure at room temperature, nano-onion carbon with diamond inside (the core is nano-diamond, and the shell is graphite spherical layer) is prepared under this condition. For specific high-resolution electron microscope pictures, see figure 1 .

Embodiment 2

[0023] Using the same raw materials as in Example 1, the powder sample was compressed and formed using the same assembly as in Example 1, the synthesis pressure was 1.0GPa, the synthesis temperature was 1373K, and the holding time was 15 minutes. After the heating was stopped, the sample was naturally cooled to room temperature. Unloading, under this condition, the complete quasi-spherical nano-onion carbon was prepared. For specific high-resolution electron microscope pictures, see figure 2 .

Embodiment 3

[0025] Using the same raw materials as in Example 1, the powder sample was compressed and formed using the same assembly as in Example 1, the synthesis pressure was 1.0GPa, the synthesis temperature was 1673K, and the pressure holding time was 15 minutes. After the heating was stopped, the sample was naturally cooled to room temperature. decompression. Nano-onion carbon with hollow polyhedral structure was synthesized under this condition. For specific high-resolution electron microscope pictures, see image 3 . From Examples 1 to 3, it can be seen that under a certain pressure and holding time, as the temperature rises, nano-diamond → nano-onion carbon containing diamond → complete quasi-spherical nano-onion carbon → nano-onion carbon with hollow polyhedral structure will occur. The transformation of onion carbon.

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Abstract

The invention discloses a high-temperature and high-pressure preparation method of carbon nano onions, and belongs to the technical field of nanomaterial preparation. The method comprises the preparation process: pressing a nano diamond powder into a cylindrical shape according to the size of a synthetic cavity, loading the cylindrical raw material obtained through cold pressing into a heating container, putting into the synthetic cavity, and at the pressure of 1.0-5.2 GPa and the temperature of 1273-1773 K, carrying out heat preservation and pressure preservation for 1-90 minutes; and finally, cooling and relieving the pressure, and thus obtaining a block carbon nano onions material. The method has the advantages of simple technological process, short preparation period, and high yield and purity; the product particle size can be controlled through the size of the raw materials; the carbon nano onions with different morphologies can be prepared through controlling the temperature, the heat preservation time and the pressure. The carbon nano onions prepared by the method have a porous structure, so the specific surface area is increased; and the prepared carbon nano onions contain oxygen-containing functional groups, so the hydrophilicity is increased.

Description

technical field [0001] The invention belongs to the technical field of nano-onion carbon preparation, and relates to a high-temperature and high-pressure preparation method of nano-onion carbon. Background technique [0002] Nano-onion carbon is nested by concentric graphite spheres. It is a member of the fullerene family and belongs to the allotrope of carbon. Nano-onion carbon has a large specific surface area, high electrical conductivity, good mechanical stability, thermal stability and electrochemical stability. These excellent physical and chemical properties make it have good application prospects in many fields, such as lithium batteries, fuel cells, dye-sensitized solar cells, supercapacitors, electrochemical hydrogen storage, microwave absorption, lubrication, catalysis and other fields. Since the discovery of nano-onion carbon in 1992, a variety of preparation methods have been invented for more than 20 years, including arc discharge, electron beam radiation, che...

Claims

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Application Information

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IPC IPC(8): B01J3/06
CPCB01J3/06B01J2203/0625
Inventor 朱品文郑艳彬陶强崔田
Owner JILIN UNIV