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Phosphorus doped graphene and preparation method thereof

A phosphorus-doped graphene and graphite technology, applied in the field of phosphorus-doped graphene and its preparation, can solve the problems of narrow adjustable range of phosphorus content, low content of phosphorus element, not very sufficient, etc., to achieve excellent electrical conductivity, process Simple, easy-to-operate effects

Active Publication Date: 2014-01-15
OCEANS KING LIGHTING SCI&TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the research on the preparation method of doped graphene is not very sufficient, and most of them focus on the research of nitrogen-doped graphene and boron-doped graphene. Phosphorus-doped graphene is relatively rare, and the reported phosphorus-doped graphene The content of phosphorus in alkenes is low, and the adjustable range of phosphorus content is narrow

Method used

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Examples

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preparation example Construction

[0021] The invention provides a kind of preparation method of phosphorus-doped graphene, comprises the following steps:

[0022] First, take graphite oxide and phosphorus pentoxide and mix them uniformly in the reactor in a mass ratio of 1:0.5~3; then, pass protective gas into the reactor, and the flow rate of the protective gas is 200-400ml / min; then, raise the temperature in the reactor to 800-900℃ at a heating rate of 15-20℃ / min, and keep it for 30min-2h; finally, at a flow rate of 200-400ml / min The temperature was lowered to room temperature in an inert gas to prepare phosphorus-doped graphene.

[0023] The protective gas is at least one of argon, nitrogen and helium.

[0024] The reactor is a tube furnace.

[0025] The mass ratio of the graphite oxide to phosphorus pentoxide is 1:1-2.

[0026] Described graphite oxide adopts following steps to make:

[0027] Add graphite to the mixed acid solution composed of concentrated sulfuric acid and concentrated nitric acid to ...

Embodiment 1

[0038] A preparation method of phosphorus-doped graphene, comprising the following steps:

[0039]Add 1g of graphite with a purity of 95% into 24ml of concentrated nitric acid with a mass fraction of 65% and 90ml of concentrated sulfuric acid with a mass fraction of 98%. The mixture is placed in an ice-water mixing bath and stirred for 20 minutes, then slowly Add potassium permanganate to the mixture, the mass ratio of potassium permanganate to graphite is 5:1, stir for 1 hour, then heat the mixture to 85°C for 30min, then add deionized water and keep at 85°C for 30min , the liquid-solid ratio of deionized water and graphite is 90ml: 1g, finally add the hydrogen peroxide solution that mass fraction is 30%, the liquid-solid ratio of hydrogen peroxide solution and graphite is 10ml: 1g, stir 10min, the mixture is pumped Filter, then wash the solid matter with dilute hydrochloric acid and deionized water successively, the solid-to-liquid ratio of dilute hydrochloric acid, deionize...

Embodiment 2

[0042] A preparation method of phosphorus-doped graphene, comprising the following steps:

[0043] 5g of graphite with a purity of 90% was added into 100ml of concentrated nitric acid with a mass fraction of 68% and 350ml of concentrated sulfuric acid with a mass fraction of 80%. Add potassium permanganate to the mixture, the mass ratio of potassium permanganate and graphite is 4:1, stir for 1 hour, then heat the mixture to 85°C for 30min, then add deionized water and continue to maintain at 85°C for 30min , the liquid-solid ratio of deionized water and graphite is 60ml: 1g, finally add the hydrogen peroxide solution that mass fraction is 30%, the liquid-solid ratio of hydrogen peroxide solution and graphite is 5ml: 1g, stir 10min, the mixture is pumped Filter, then wash the solid matter with dilute hydrochloric acid and deionized water successively, the solid-to-liquid ratio of dilute hydrochloric acid, deionized water and graphite is 90ml: 60ml: 1g, wash altogether 3 times, ...

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Abstract

The invention provides a preparation method for phosphorus doped graphene. The preparation method comprises the following steps: uniformly mixing graphite oxide and phosphorus pentoxide in a mass ratio of 1: 0.5-3 and placing an obtained mixture in a reactor; introducing protective gas into the reactor, wherein introduction flow velocity of the protective gas is 200 to 400 ml / min; heating the interior of the reactor to a temperature of 800 to 900 DEG C at a heating speed of 15 to 20 DEG C / min and maintaining the temperature for 30 min to 2 h; and cooling the reactor to room temperature in the protective gas with flow velocity of 200 to 400 ml / min so as to prepare the phosphorus doped graphene. According to the method, phosphorus pentoxide is used as a phosphorus source, the maximum doping amount of elemental phosphorus can approach 10%, so the adjustable range of phosphorus is wide; and the method has the advantages of simple process, convenient operation, no special requirements on equipment and easy realization of large scale industrial production. The invention further provides the phosphorus doped graphene prepared by using the preparation method.

Description

technical field [0001] The invention relates to the field of material synthesis, in particular to a phosphorus-doped graphene and a preparation method thereof. Background technique [0002] Graphene is a two-dimensional carbon atom crystal discovered by Andre K. Geim of the University of Manchester in 2004. It is a single-layer or multi-layer extremely thin carbon material. Single-layer graphene has excellent electrical and thermal conductivity and low thermal expansion coefficient, and its theoretical specific surface area is as high as 2630m 2 / g (A Peigney, Ch Laurent, et al. Carbon, 2001, 39, 507), can be used in effect transistors, electrode materials, composite materials, liquid crystal display materials, sensors, etc. [0003] At present, the methods for preparing graphene mainly include graphite exfoliation (Novoselov K S, Geim A K, et al. Science 2004, 306, 666), chemical redox method [D A Dikin, et al. Nature 2007, 448, 457; Sasha Stankovich, Dmitriy A Dikin, Ric...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04C01B32/184C01B32/194
Inventor 周明杰钟辉王要兵
Owner OCEANS KING LIGHTING SCI&TECH CO LTD
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