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Amido reinforced graphene film, nitrogen doped graphene film and preparation method thereof

A nitrogen-doped graphene and graphene film technology, applied in the field of amine-based reinforced graphene films, can solve the problems of limiting large-scale and continuous preparation of graphene films, difficult to disperse, coordinate and solidify, and impossible to solidify and form. , to achieve the effect of easy operation, simple operation and low cost

Active Publication Date: 2016-10-19
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003]Macroscopically assembled graphene film is a main form of macroscopic nano-scale graphene sheets. Commonly used methods include suction filtration, scraping film, and spin coating and spraying methods, etc., but these methods limit the large-scale and continuous preparation of graphene films
Chinese invention patent CN201410457039.6 discloses two methods for preparing graphene membranes: firstly, by wet spinning, the membranes are precipitated in a coagulation solution such as an inorganic metal salt solution, dried, and then reduced by a reducing agent. One-step preparation of ion-enhanced graphene membranes, although this method provides a method for continuous preparation of graphene membranes by wet spinning, the preparation process is cumbersome, two-step methods are required to achieve graphene membranes, and due to the precipitation of inorganic salt ions The defect that remains in the film after the agent is added, and the heat treatment process cannot remove it; secondly, the graphene solution is used as the raw material, and the film is solidified in the coagulation solution containing the coordination ions, and dried to obtain the ion-enhanced graphene film. Although the preparation method is simple, because graphene itself has no special functional groups, it is difficult to disperse in organic solvents or water and coordinate solidification with coordination ions, and the concentration of the solution is also difficult to reach the concentration required for solidification. , so it is basically impossible to solidify the graphene solution as the raw material in the coordination ion coagulation solution

Method used

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  • Amido reinforced graphene film, nitrogen doped graphene film and preparation method thereof
  • Amido reinforced graphene film, nitrogen doped graphene film and preparation method thereof
  • Amido reinforced graphene film, nitrogen doped graphene film and preparation method thereof

Examples

Experimental program
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Embodiment 1

[0035] The preparation method of graphene oxide solution:

[0036] Add 10g of graphite, 150ml of 98% sulfuric acid, and 30ml of nitric acid into a 500ml Erlenmeyer flask and stir at room temperature for 24 hours, slowly pour it into 1L of water to collect the solid, wash it 3 times, and dry it at 80°C for 4 hours. Repeat the pre-oxidation process twice. The dried pre-oxidized graphite was put into a box furnace and thermally expanded at 900°C for 20s to obtain thermally expanded graphite oxide. In a 500ml wide-mouth Erlenmeyer flask, mix 5g of heat-expandable graphite oxide with 300ml of sulfuric acid, 5g of K 2 S 2 o 8 , 7g of phosphorus pentoxide mixed and heated at 80°C for 4 hours, diluted with 2L of water, filtered and washed, dried in air for 3 days to obtain pre-oxidized thermally expandable graphite. Mix dry pre-oxidized heat-expandable graphite with 200ml of sulfuric acid at a low temperature of 0-5°C, add 20g of potassium permanganate, add slowly, stir at 35°C fo...

Embodiment 2

[0039] The preparation method of graphene oxide solution is as embodiment 1.

[0040] Extrude a 30mg / mL graphene oxide solution at a extrusion speed of 10mL / h in a device with a flat inline die, with a die height of 100μm and an aspect ratio > 5, in ethylenediamine at 60°C and sodium citrate mixed solution (the mass fraction of ethylenediamine is 20%, the mass fraction of sodium citrate is 20%), stay in 8h, solidify and form a film by reducing self-assembly, and obtain amine-based reinforced graphite after drying at 85°C for 4h olefin film; wherein, the percentage is the mass percentage of each component relative to the mixed liquid. The thickness, tensile strength, elongation at break and electrical conductivity of the obtained amine-based reinforced graphene film are shown in Table 1.

Embodiment 3

[0042] The preparation method of graphene oxide solution is as embodiment 1.

[0043] Extrude 10mg / mL graphene oxide solution at a rate of 100mL / h through a device with a flat inline die. The die height is 500 μm and the aspect ratio is >5. The mixed solution of ethylene tetramine and sodium bisulfite (the mass fraction of ammonia water is 30%, the mass fraction of triethylene tetramine is 5%, the mass fraction of sodium bisulfite is 40%) stays in 24h, self-assembles by reduction Solidify into a film, and dry at 75°C for 12 hours to obtain an amine-reinforced graphene film; wherein, the percentages are the mass percentages of each component relative to the mixed solution. The thickness, tensile strength, elongation at break and electrical conductivity of the obtained amine-based reinforced graphene film are shown in Table 1.

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Abstract

The present invention discloses an amido reinforced graphene film, a nitrogen doped graphene film and a preparation method thereof. The method includes the following steps: extruding a graphene oxide solution by a device with an in-line die orifice nozzle; staying, solidifying and reducing in a mixed liquid of liquid amine solidification liquid and a reducing agent for self-assembly into a film, and drying, wherein the temperature of the mixed liquid is 60-95 DEG C, and the stay time is more than 0.5 h. The method has the wide raw material sources and low cost; the preparation method uses graphene oxide solution as raw material, realizes solidification, reduction and self-assembly into amido reinforced graphene film through one step, has the advantages of low reaction temperature, simple operation, green and environment-friendliness, and can realize large-scale continuous preparation. The amido reinforced graphene film prepared by the method has good strength and toughness, excellent thermal conductivity and electrical conductivity, and broadens the scope for subsequent application. The amido reinforced graphene film can increase the electrical conductivity and mechanical properties of the film.

Description

technical field [0001] The field relates to an amine-based reinforced graphene film, a nitrogen-doped graphene film and a preparation method thereof. Background technique [0002] As the most basic structural unit of all carbon materials, graphene has a true single atomic layer thickness and strict two-dimensional structure, and has high mechanical strength, elasticity, thermal conductivity, electrical conductivity, and quantum Hall effect. Since British scientists (Andre Geim) Andre Geim and (Konstantin Novoselov) Kostyanovosenov discovered graphene and won the Nobel Prize in 2010, the research on graphene has reached an unprecedented climax, and more and more Studies have found that it has great application prospects in special fields such as energy storage, electrical devices, catalysis, and biomedicine. [0003] The macroscopically assembled graphene film is a main form of macroscopic nanoscale graphene sheets. The commonly used methods include suction filtration, scrap...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04
Inventor 李吉豪李景烨李林繁张阔贾娜
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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