Thermal preparation method of solution of self-supported porous graphene-based membrane

A porous graphene and graphene-based technology, applied in the field of graphene-based film preparation, can solve the problems of poor electrochemical performance, limited size and thickness of self-supporting graphene-based films, etc., and achieve the effect of improving specific capacitance value

Active Publication Date: 2014-12-10
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention aims to solve the technical problems that the existing self-supporting graphene-based film is limited in size and thickness, and the serious recombination between graphene sheets du

Method used

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  • Thermal preparation method of solution of self-supported porous graphene-based membrane
  • Thermal preparation method of solution of self-supported porous graphene-based membrane
  • Thermal preparation method of solution of self-supported porous graphene-based membrane

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specific Embodiment approach 1

[0061] Embodiment one: the solution thermal preparation method of the self-supporting porous graphene-based film of the present embodiment is carried out according to the following steps:

[0062] 1. The concentration of graphite oxide is 0.01mg·mL -1 ~0.5mg·mL -1 , adding graphite oxide into water, ultrasonically exfoliating and dispersing for 0.5-10 hours under ultrasonic conditions with a frequency of 20-100KHz, to obtain a graphene oxide aqueous dispersion;

[0063] 2. Under the condition that the temperature is 20° C. to 100° C., the graphene oxide aqueous dispersion obtained in step 1 is evaporated under reduced pressure or evaporated at normal pressure to concentrate;

[0064] 3. Spread the graphene oxide aqueous dispersion concentrated in step 2 to form a film on the flat substrate, and after drying at room temperature, peel off the film from the substrate to obtain a graphene oxide film;

[0065] 4. According to the solute concentration of 0.01mol L -1 ~20mol·L -1...

specific Embodiment approach 2

[0067] Specific embodiment two: the difference between this embodiment and specific embodiment one is that the preparation method of graphite oxide described in step one is as follows: in a dry beaker, add 120mL of H with a mass percentage concentration of 98% 2 SO 4 , then place the beaker in an ice-water bath, add 5g graphite and 2.5g NaNO 3 , stirring at a speed of 50-500 rpm, while gradually adding 15g of powdered KMnO 4 , continue to react for 2 hours in an ice-water bath and stirring; move the beaker into a constant temperature oil bath at 35±1°C and continue to react for 2 hours; slowly add 360mL of distilled water under stirring at a speed of 50 to 500 rpm, and control the temperature to be constant At 75°C, continue the constant temperature reaction for 1h; add 1000mL of distilled water at a temperature of 40°C, add 50mL of hydrogen peroxide with a concentration of 30% by mass, and then vacuum filter; wash the filter cake with hydrochloric acid with a concentration o...

specific Embodiment approach 3

[0069] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is that the decompression evaporation described in step two has a temperature of 40°C to 90°C, a vacuum degree of -0.07MPa to -0.1Mpa, and a rotation speed of 20 RPM~500 RPM rotary evaporation under reduced pressure. Others are the same as in the first or second embodiment.

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Abstract

The invention relates to a thermal preparation method of a solution of a self-supported porous graphene-based membrane, relates to a preparation method of a self-supported porous graphene-based membrane, and aims to solve the technical problems that the size and the thickness of a conventional self-supported porous graphene-based membrane are limited and the electrochemical performance of the conventional self-supported porous graphene-based membrane is poor caused by severe interlay lamination of graphene sheets in the chemical reduction process. The thermal preparation method comprises the following steps: dispersing graphene oxide into water, adding or not adding a doped carbon material, concentrating, and spreading into a membrane, thereby obtaining a graphene oxide membrane; preparing a thermal treatment solution by using acid or alkali solute, putting the graphene oxide membrane into a reaction kettle with a polytetrafluoroethylene lining, adding the thermal treatment solution according to the standard that the membrane is submerged, sealing the reaction kettle, and subsequently performing thermal treatment, thereby obtaining the self-supported porous graphene-based membrane. The self-supported porous graphene-based membrane is prepared by orderly arranging graphene sheets in parallel, and due to the gaps among the graphene sheet layers, the self-supported porous graphene-based membrane can be used in electrochemical energy storage devices such as supercapacitors.

Description

technical field [0001] The invention relates to a preparation method of a graphene-based thin film. Background technique [0002] Supercapacitor is a new type of electrochemical energy storage device, which has the advantages of ultra-high-speed charge and discharge capacity, ultra-long cycle life, and good high and low temperature performance. It is suitable for a wide range of fields such as electric vehicle power supply, energy storage power supply, and electronic equipment power supply. Among them, wearable and windable flexible supercapacitors are particularly concerned by the market. In order to improve the energy density of supercapacitors and realize the coilability of supercapacitors, the use of self-supporting graphene-based films as current collector-free and binder-free electrodes of supercapacitors has become a current research hotspot. [0003] The preparation methods of self-supporting graphene-based film materials used as supercapacitor electrode materials m...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 贾铮李程远刘道庆
Owner HARBIN INST OF TECH
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