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Method for quickly preparing large-area graphene foam/polymer fiber three-dimensional network composite foam film

A technology of graphene foam and three-dimensional network, applied in the direction of graphene, chemical instruments and methods, synthetic resin layered products, etc., can solve the difficulty of obtaining large-area high-mechanical-strength graphene composite films, control problems of equipment and conditions Relatively harsh, difficult to control film thickness and other issues, to achieve the effect of short preparation cycle, good mechanical properties and high mechanical strength

Inactive Publication Date: 2014-03-12
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chemical vapor deposition is a method that is widely used at present, and can obtain a continuous graphene film with uniform thickness, but this method is affected by many factors, such as the choice of carbon source, the chemical properties and surface properties of the substrate material, And there are more stringent requirements for the control of equipment and conditions
The composite membrane of graphene and polymer nanofibers obtained by microfiltration with microporous membranes is more serious, and it is difficult to obtain a graphene composite membrane with large area and high mechanical strength, and the filtration speed is slow and the cycle is long.
Drip coating, spray coating and casting methods waste a lot of solvent and it is difficult to control the film thickness

Method used

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  • Method for quickly preparing large-area graphene foam/polymer fiber three-dimensional network composite foam film
  • Method for quickly preparing large-area graphene foam/polymer fiber three-dimensional network composite foam film
  • Method for quickly preparing large-area graphene foam/polymer fiber three-dimensional network composite foam film

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] like figure 1 Shown:

[0022] The first step is the preparation of graphene oxide hydrosol, and the specific steps are:

[0023] Step (1). Add 2g flake graphite powder in four-necked flask, 20mL concentrated H 2 SO 4 , 2g K 2 S 2 o 8 , and 1g P 2 o 5 ;Stir for 4 hours at a temperature of 65°C, dilute the mixture with deionized water, filter and wash, and dry the filter cake at 50°C;

[0024] Step (2). 30mL concentrated H 2 SO 4 , 40 mL concentrated H 3 PO 4 , 2g of dry filter cake was added to a four-necked flask, and mechanically stirred; when the temperature of the mixture in the four-necked flask was lower than 20°C, 3g of NaNO was added under stirring 3 and 5g KMnO 4 , stirred for 10 min; heated to 30 ° C, stirred for 3 h; slowly added 100 mL of deionized water; and 10 mL of 30% H 2 o 2 , to obtain bright yellow solution, continue to stir for 2h;

[0025] Step (3). After the reaction, the bright yellow solution is centrifuged and washed 6 times with ...

Embodiment 2

[0039] The first step is the preparation of graphene oxide hydrosol, and the specific steps are:

[0040] Step (1). Dissolve 30mL of concentrated H under ice bath conditions 2 SO 4 , 40 mL concentrated H 3 PO 4 , Add 2g flake graphite powder into the four-necked flask and stir mechanically; when the temperature of the mixture in the four-necked flask is lower than 20°C, add 3g NaNO 3 and 5g KMnO 4 , stirred for 10 min; warmed up to 40 ° C, stirred for 2 h; slowly added 200 mL of deionized water; heated to 75 ° C, continued to stir for 60 min; added 15 mL of 30% H 2 o 2 , to obtain bright yellow solution, continue to stir for 1.5h;

[0041]Step (2). After the reaction, the bright yellow solution is centrifuged and washed 8 times with 5% HCl solution by mass fraction, and then centrifuged and washed with deionized water until the supernatant is neutral, and the centrifuge speed is 10000 rpm , and then concentrate the graphene oxide aqueous solution to finally obtain a gra...

Embodiment 3

[0054] The first step is the preparation of graphene oxide hydrosol, and the specific steps are:

[0055] Step (1). Add 2g flake graphite powder in four-necked flask, 20mL concentrated H 2 SO 4 , 2g K 2 S 2 o 8 , and 1g P 2 o 5 ;Stir for 3 hours at a temperature of 70°C, dilute the mixture with deionized water, filter and wash, and dry the filter cake at 60°C;

[0056] Step (2). 30mL concentrated H 2 SO 4 , 40 mL concentrated H 3 PO 4 , 2g of dry filter cake was added to a four-necked flask, and mechanically stirred; when the temperature of the mixture in the four-necked flask was lower than 20°C, 3g of NaNO was added under stirring 3 and 5g KMnO 4 , stirred for 10 min; heated to 45 ° C, stirred for 1 h; slowly added 150 mL of deionized water; heated to 80 ° C, continued to stir for 50 min; added 20 mL of 30% H 2 o 2 , to obtain bright yellow solution, continue to stir for 1h;

[0057] Step (3). After the reaction, the bright yellow solution is centrifuged and wa...

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Abstract

The invention relates to a method for quickly preparing a large-area graphene foam / polymer fiber three-dimensional network composite foam film. The method mainly comprises the processes of preparation of high-viscosity graphene oxide hydrosol, film formation by rolling, drying and reduction to finally obtain the large-area graphene foam / polymer fiber three-dimensional network composite foam film. The method has the technical effects that the graphene foam / polymer fiber three-dimensional network composite foam film which is controllable in thickness, large-area, high in mechanical strength, high in conductivity, light in weight and high in porosity and has certain elasticity is prepared. The composite film is similar to foam, is a self-supported flexible film, and can be bent and folded; the thickness of the composite film is 5 to 10 times that of a graphene oxide composite film prior to reduction; in the preparation process, expensive equipment and severe conditions are not needed; the composite film is easy to operate, low in cost, short in preparation period and simple in experiment condition, and industrial production can be realized.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of graphene materials, and in particular relates to a rapid preparation method of a graphene foam / polymer fiber three-dimensional network composite foam film. Background technique [0002] Graphene is a two-dimensional planar single-atom-layer-thick hexagonal arrangement of carbon materials, also known as single-layer graphite. 15000cm 2 / V·s, the resistivity is only 10 -6 Ω·cm. Graphene has excellent electrochemical properties and high theoretical specific surface area. In addition, large-area graphene films also have good flexibility, and have important applications in portable electronic devices and flexible electronic devices. High-porosity graphene foam membranes have potential applications in catalyst support materials and fuel cell electrode materials. However, it is currently difficult to prepare large-area, high mechanical strength, and high porosity flexible graph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B32B37/06B32B27/02B32B9/04B32B5/18C01B31/04C01B32/184
Inventor 肖启振罗忠平
Owner XIANGTAN UNIV
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