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Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock

A metal particle and graphene technology, which is applied in the field of high-temperature thermal shock preparation of coal-based graphene-loaded metal particles, can solve the problems of high energy consumption, long reaction time, and high cost of solvothermal reaction, and achieve rapid response, low cost, and The effect of cheap raw materials

Active Publication Date: 2021-09-03
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, all of these methods use expensive graphene oxide or reduced graphene oxide as precursors, and use solvothermal reaction with high energy consumption and long reaction time. Moreover, these synthesis techniques require two or more Complicated synthesis steps [CN201611108184.9], the process is relatively complicated
[0007] At present, the method of preparing coal-based graphene loaded with metal nanoparticles by one-step high-temperature thermal shock method has not been reported.

Method used

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  • Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock
  • Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock
  • Method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] High-temperature thermal shock of coal-based graphene supported metal Ni under different discharge voltages:

[0028] Step 1) preparation takes by weighing excessive nickel chloride hexahydrate NiCl with analytical balance 2 · 6 h 2 O, 20g dissolved in a small amount of water H 2 O, 5mL, prepare supersaturated NiCl 2 aqueous solution;

[0029] Step 2) Add 200 mesh 1g coal tar pitch, mix the solution evenly, let stand, filter and dry to obtain conductive NiCl 2 @Coal tar pitch precursor;

[0030] Step 3) Accurately weigh 120mg of dried and processed NiCl 2 @Coal tar pitch precursor, put the sample in a quartz tube with an inner diameter of 6mm, and fix the loaded quartz tube at both ends of the capacitor electrode;

[0031] Step 4) Set inert gas protection, vacuumize the reaction chamber with a vacuum pump and fill it with nitrogen, repeat three times to replace the oxygen in the reaction chamber to ensure that the materials are not oxidized during the reaction. ...

Embodiment 2

[0035] High-temperature thermal shock of metal Ni supported on coal-based graphene under different discharge times:

[0036] Step 1)-4) with embodiment 1;

[0037] Step 5) Apply high voltage, choose capacitor 60mF, choose voltage 200V, power-on time is 50ms, 100ms, 150ms, 200ms, 300ms, sieve the coal-based graphene material that is less than 200 meshes and load metal nanoparticles.

[0038] like figure 1 Shown is a comparison chart of Raman spectra of coal-based graphene loaded with metal Ni nanoparticles before and after high temperature thermal shock in Examples 1 and 2. Among them, (a) is NiCl before flashing 2 @The Raman spectrum of the coal tar pitch precursor, (b)-(e) is the comparison figure of the Raman spectrum of the coal-based graphene loaded with metal Ni nanoparticles after different voltage treatments in Example 1, (f) is different Voltage I D / I G and I 2D / I G The ratio of; (g)-(k) is the contrast figure of the Raman spectrum of the coal-based graphene o...

Embodiment 3

[0042] High-temperature thermal shock of coal-based graphene-supported metal Co:

[0043] Step 1) preparation takes by weighing excessive cobalt chloride hexahydrate CoCl with analytical balance 2 · 6 h 2 O, 20g dissolved in a small amount of water H 2 O, 5mL, prepare supersaturated CoCl 2 aqueous solution;

[0044] Step 2-4 is with embodiment 1;

[0045] Step 5) Apply a high voltage, select a capacitor of 60mF, select a voltage of 200V, and a power-on time of 200ms, and sieve out a coal-based graphene material with a mesh size of less than 200 to obtain metal nanoparticles.

[0046] like Figure 4 Shown is the scanning electron microscope image of the coal-based graphene loaded with metal Co nanoparticles after high temperature thermal shock in Example 3. It can be seen from the figure that the metal Co particles are successfully loaded on the graphite sheet after high temperature thermal shock.

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Abstract

The invention provides a method for preparing metal particle-loaded coal-based graphene through high-temperature thermal shock. Nano metal particles are introduced into a carbon source through a dipping reduction method. According to the method, the carbon sources such as coal, coal pitch, coke and coal-based graphite are subjected to high-temperature thermal shock graphitization and metal salt thermal reduction by utilizing joule heat generated by capacitor discharge, and the coal-based graphene-loaded metal particles are generated in a short time. The metal used in the metal nano particle loading process is transition-state metal such as Fe, Co, Ni and Cu, and the metal salt is one of chloride or hydrate thereof, acetate or hydrate thereof. The preparation method is simple, low in cost, high in product graphitization degree, excellent in performance and suitable for large-scale production and has important application value.

Description

technical field [0001] The disclosure relates to the field of material preparation, in particular to a method for preparing coal-based graphene-supported metal particles by high-temperature thermal shock. Background technique [0002] Supercapacitors have high power density, but they generally have lower energy density than rechargeable batteries. Therefore, supercapacitors with higher operating voltage and higher energy density without sacrificing power transmission and cycle life have been developed to meet the energy storage demand in the rapidly growing world. [0003] Pseudocapacitors can make full use of the different potential windows of the two electrodes to provide the maximum operating voltage in battery systems, leading to greatly improved specific capacitance and significantly enhanced energy density. Metal hydroxides and conducting polymer materials are excellent electrode materials for pseudocapacitors due to outstanding theoretical capacitance and abundant an...

Claims

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Application Information

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IPC IPC(8): B22F9/30B22F1/00C01B32/184H01G11/32H01G11/44B82Y30/00B82Y40/00
CPCB22F9/30B82Y30/00B82Y40/00C01B32/184H01G11/32H01G11/44C01B2204/22Y02E60/13
Inventor 朱荣涛黄鹏飞章新喜张文军刘壮朱海洋廖云天吴雨
Owner CHINA UNIV OF MINING & TECH
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