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Nitrogen-doped porous graphite and preparation method thereof

A technology of porous graphene and nitrogen doping, applied in the field of nanomaterials, can solve the problems of difficult large-scale preparation, complex preparation process, destruction of two-dimensional structure, etc., and achieve the effects of easy satisfaction of method conditions, low process cost, and simple process.

Inactive Publication Date: 2016-06-01
SHANGHAI JIAO TONG UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, these methods often have the following obvious disadvantages: complex preparation process, difficult large-scale preparation, high cost, wide pore size distribution, small specific surface area (usually less than 1000m 2 g -1 ), or the re-agglomeration seriously destroys the original two-dimensional structure and other shortcomings
XPwang et al. published High-DensityMonolithofN-DopedHoleyGrapheneforUltrahighVolumetricCapacityofLi-IonBatteries in the journal AdvancedEnergyMaterials in 2016. They studied a "top-down" method for preparing nitrogen-doped porous graphene. First, porous graphene oxide was obtained by etching graphene oxide with hydrogen peroxide. Nitrogen-doped porous graphene is obtained by doping porous graphene with polymer at high temperature, but the nitrogen-doped porous graphene obtained has a wide pore size distribution and a specific surface area of ​​only 612m 2 g -1

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  • Nitrogen-doped porous graphite and preparation method thereof
  • Nitrogen-doped porous graphite and preparation method thereof
  • Nitrogen-doped porous graphite and preparation method thereof

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Embodiment 1

[0035] This embodiment relates to a method for preparing nitrogen-doped porous graphene with a high specific surface area, which is economical, scalable and has a narrow pore size distribution. The method comprises the following steps:

[0036] Dissolve zinc nitrate hexahydrate and glucose in an aqueous solution in a mass ratio of 4:1, and first react the mixed aqueous solution at 150°C in the air environment of a muffle furnace to form a zinc oxide / porous ultra-thin carbon layer / zinc oxide sandwich structure product, Scanning electron microscope picture as figure 1 shown;

[0037] Then, the ZnO / porous ultra-thin carbon layer / ZnO interlayer structure product is further graphitized in a tube furnace at a heating rate of 10°C / min and heated to 800°C for 5min in a non-oxidizing gas atmosphere. Wash away the zinc oxide with an aqueous acid solution.

[0038] Analysis of the nitrogen-doped porous graphene data prepared in this example shows that the pore diameter ranges from 2 to...

Embodiment 2

[0040] This embodiment relates to a method for preparing nitrogen-doped porous graphene with a high specific surface area, which is economical, scalable and has a narrow pore size distribution. The method comprises the following steps:

[0041] Dissolve zinc nitrate hexahydrate and soluble starch in an aqueous solution at a mass ratio of 4:1, and first react the mixed aqueous solution at 150°C in the air environment of a muffle furnace to form a zinc oxide / porous ultra-thin carbon layer / zinc oxide sandwich structure product ;

[0042] Then the zinc oxide / porous ultra-thin carbon layer / zinc oxide sandwich structure product is further heated in a tube furnace at a heating rate of 30°C / min, and heated to 500°C for 120min in a non-oxidizing gas atmosphere. After further graphitization, Wash away the zinc oxide with an aqueous acid solution.

[0043] Analysis of the nitrogen-doped porous graphene data prepared in this example shows that the pore size range is 2-6 nm, and the pore ...

Embodiment 3

[0045] This embodiment relates to a method for preparing nitrogen-doped porous graphene with a high specific surface area, which is economical, scalable and has a narrow pore size distribution. The method comprises the following steps:

[0046] Zinc nitrate hexahydrate and sucrose are dissolved in an aqueous solution at a mass ratio of 4:1, and the mixed aqueous solution is first rapidly reacted at 500°C in a muffle furnace air environment to form a zinc oxide / porous ultra-thin carbon layer / zinc oxide sandwich structure product;

[0047] Then, the ZnO / porous ultra-thin carbon layer / ZnO sandwich structure product is further graphitized in a tube furnace at a heating rate of 2°C / min, heated to 1700°C for 5min in a non-oxidizing gas atmosphere, and then graphitized. Wash off the zinc oxide with an aqueous acid solution.

[0048] The data analysis of the nitrogen-doped porous graphene prepared in this example shows that the pore size ranges from 2 to 6 nm.

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Abstract

The invention discloses nitrogen-doped porous graphite and a preparation method thereof. The preparation method comprises the following steps of conducting low temperature heat treatment on a mixed aqueous solution of nitrate and a carbon source, so that a metal oxide hard template-thin carbon layer precursor is formed; conducting graphitization on the obtained metal oxide hard template-thin carbon layer precursor, so that the nitrogen-doped porous graphite is obtained. According to the method, raw materials are conventional materials, process cost is low, and conditions of the method are easy to meet; the novel template method is adopted for directly pyrolyzing saccharides organic matter, so that the nitrogen-doped porous graphite is obtained, and the process is quite simple and fast; the nitrogen-doped porous graphite is quite simple in operation, low in cost, high in yield and capable of being produced on a large scale, the less-layer porous graphite which has abundant surface pores, narrow in pore size distribution and high in specific surface area can be obtained, and the nitrogen-doped porous graphite and the preparation method thereof are applicable to such fields as supercapacitors, fuel-cell catalysts, electrocatalysis, lithium batteries, adsorption and gas separation.

Description

technical field [0001] The invention relates to the technical field of nanomaterials, in particular to a nitrogen-doped porous graphene and a preparation method thereof. Background technique [0002] Since its discovery, graphene has become a research hotspot in the past ten years due to its superior performance in many aspects. However, the application of graphene still faces various difficulties. For graphene applications, its regulation of structure is crucial. Recently, a new spatial structure of graphene, porous graphene with abundant two-dimensional surface pores, can enable rapid material transport and effectively prevent graphene from re-accumulating into a graphite structure due to intermolecular forces, and a large number of accessible surfaces Defects, large specific surface area, rich surface functional groups and other advantages have attracted more attention. It has broad application prospects in supercapacitors, fuel cell catalysts, electrocatalysis, lithium...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
CPCC01P2004/03
Inventor 张亚非董新伟苏言杰
Owner SHANGHAI JIAO TONG UNIV
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