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Preparation method of graphene thin film

A graphene film and graphene technology, applied in graphene, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as poor performance, time-consuming high-temperature reduction, high energy consumption, etc., and achieve excellent performance and avoid cooling opportunities Effect

Inactive Publication Date: 2017-04-26
SOUTHEAST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Graphene films grown by chemical vapor deposition have excellent properties, but the high energy consumption and time-consuming of long-term (usually in hours) high-temperature growth limit their large-scale applications; while graphene derivative films based on graphene derivative coatings have The problem of poor performance: Graphene oxide not only has holes but also its electrical and thermal conductivity are greatly reduced due to the oxidation of its basal surface, and it is difficult to restore the principle, and the chemical reduction is polluted and high-temperature reduction is time-consuming (usually Hours) and high energy consumption; and the performance of graphene edge derivative films also needs to be improved
Generally, the heating time of a microwave oven is set in multiple levels with a unit of 30 seconds, but experiments have shown that heating a whole level under a protective atmosphere may cause the coated graphene derivative layer to be scattered or even fall off due to excessive temperature rise. The microwave oven can set the microwave pulse length, but it is also difficult to set the possible optimal heating time, such as 1.2 seconds, while the carrier compound passes through the microwave heating zone at a set speed, and the precise optimal heating time can be easily obtained according to the size of the microwave heating zone
In addition, the carrier compound is heated in a microwave oven for a period of time. After taking it out, it can be clearly felt that the carrier compound placed in different heating areas has different heating effects. This is related to the uniformity of the heating electric field in the microwave oven. Although it can be designed such as Surface antenna structure and other methods can improve the heating uniformity of microwave ovens, but it also has a certain limit

Method used

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  • Preparation method of graphene thin film
  • Preparation method of graphene thin film

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Experimental program
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Effect test

Embodiment 1

[0027] First, graphene oxide powder and reduced graphene oxide powder are prepared. 30 grams of graphite mixed with 15 grams of sodium nitrate and 750 milliliters of concentrated sulfuric acid. The mixture was cooled to 0°C in an ice bath, and after stirring for 2 h, 90 g of potassium permanganate was slowly added, keeping the temperature of the mixture below 5°C during the mixing process. The mixture was stirred for another hour and allowed to warm to room temperature by removing the ice bath. Add 1 liter of distilled water to the mixture and increase the temperature in the oil bath to 90°C. Another 300 ml of water were added and stirred for another hour and a half. The color of the mixture turned brown. The mixture was then treated and diluted with 30% hydrogen peroxide in 300 ml and 30 liters of hot water. The mixture was further washed with excess water until the pH of the filtrate was almost neutral to obtain graphene oxide. Then graphene oxide was dispersed in water...

Embodiment 2

[0030] First obtain dust-free asbestos paper with a thickness of 1 mm, a length of 1 meter, and a width of 0.5 meters. Then soak the dust-free asbestos paper in a 10 mg / ml graphene oxide aqueous solution for 5 minutes, then take it out and dry it in the air to obtain a composite asbestos paper coated with a graphene oxide layer on the surface. The composite asbestos paper was treated in hydrazine hydrate vapor at 95 degrees Celsius for 24 hours to reduce the graphene oxide layer to obtain the composite asbestos paper coated with the reduced graphene oxide layer. Then, under the protection of nitrogen at room temperature, the composite asbestos paper is driven by a high-temperature conveyor belt at a speed of 0.05 m / s to pass through a heating zone with a width of 0.5 meters and a length of 0.1 meters constructed by five microwave ovens with a power of 1000W for about 2 seconds. The composite asbestos paper enters the room temperature area for cooling, repeats the microwave hea...

Embodiment 3

[0032] First, obtain an alkali-free glass fiber cloth with a thickness of 0.1 mm and a width of 10 cm with a warp and latitude of 47.4*27.5. Then the non-alkali glass fiber cloth is passed through a 30 cm long 1 mg / ml reduced graphene oxide aqueous solution at a speed of 0.01 m / s, and after drying, a composite non-alkali glass fiber cloth coated with a reduced graphene oxide layer is obtained. Under the protection of helium, the composite non-alkali glass fiber cloth is heated at a speed of 0.05 m / s at room temperature by a microwave oven with a power of 1000W and a heating area with a diameter of 10 cm for about 2 seconds, then enters the room temperature area again for cooling, and repeats The above microwave heating-cooling process was performed 5 times, and then the composite non-alkali glass fiber cloth was extruded through extrusion rollers with a line pressure of 1300 N / cm to obtain a carbon content greater than 90% and an electrical conductivity greater than 5000Sm -1 ...

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Abstract

The invention discloses a preparation method of a graphene thin film. A graphene derivative and inorganic non-metal plane carrier composite material passes through a microwave heating region at a set speed for the first time so as to precisely control the heating time and the cooling chance, so that heating nonuniformity caused by difference among different regions of microwave heating is inhibited and mechanical continuous production is easily realized; moreover, a microwave technology capable of heating quickly and a microwave absorption characteristic and a high heat conducting capacity of the graphene derivative are combined, and meanwhile, by virtue of the characteristics that the inorganic non-metal plane carrier is high-temperature resistant and heat of the surface graphene derivative layer is easily and quickly exchanged and transferred, the graphene derivative layer coated on the surface of a carrier can be quickly converted into a graphene layer, and then the graphene layer and the carrier are separated to obtain the graphene thin film which has a good electric conducting ability. The graphene thin film prepared by the method is excellent in performance and can make contribution to further development and application of conductive thin films and graphene materials.

Description

technical field [0001] The invention belongs to the field of materials, and relates to a graphene film, especially by using the characteristics of rapid microwave heating and the microwave absorption characteristics and high thermal conductivity of graphene derivatives. The surface of the carrier is formed by coating the surface of an inorganic non-metallic plane carrier with a solution of graphene derivatives. Coating the composite of the graphene derivative layer, then the composite moves through the microwave heating zone at a set speed and selectively heats the graphene derivative layer in the microwave heating zone and then rapidly cools and extrudes to obtain a good A carrier composite covered by a graphene layer with conductivity, and a graphene film can be obtained by separating the graphene layer and the carrier. Background technique [0002] With the development of society, thin films have a wide range of application values ​​in fields including sealing, sensing, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/184
CPCC01B2204/22C01B2204/24C01B2204/30
Inventor 张继中
Owner SOUTHEAST UNIV
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