Rapid growth method of large-sized graphene glass

A growth method and graphene technology, applied in graphene, nano-carbon, metal material coating processes, etc., can solve the problems of uneven layer thickness, limited size, weak cracking ability, etc., and achieve concentration distribution and airflow distribution. Uniformity, ensuring uniformity, and enhancing the effect of concentration

Active Publication Date: 2018-01-05
北京石墨烯研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The liquid phase coating method is an early method for the preparation of graphene-glass composite materials. The size of graphene sheets is small, with many defects and uneven layer thickness, resulting in poor quality of graphene films prepared by this method. Difficult to realize its practical application
The transfer preparation method is a commonly used method for preparing graphene-glass composites. However, the pollution and damage caused by graphene during the transfer process are unavoidable, which significantly reduces the performance of graphene.
At the same time, graphene and glass are only combined by a weak van der Waals force, and the transferred graphene film is easy to fall off and damage from the glass, making it difficult to maintain its stable performance, and can hardly be used for the development of actual products.
The technical bottlenecks in the direct growth of graphene on the glass surface are: on the one hand, the ability of glass itself to catalyze the cracking of carbon precursors is very weak, and the carbon precursors mainly rely on thermal cracking, which makes it difficult for graphene to nucleate and grow on the glass surface; On the one hand, the softening temperature of glass itself is generally lower than the growth temperature of graphene, which limits the growth process of graphene (the growth temperature is lower than that on metal substrates)
The developed graphene glass atmospheric pressure (AP) CVD preparation technology mainly has two disadvantages: 1) The growth time of graphene is too long, generally takes several hours to more than ten hours, the production efficiency is low, and the energy consumption is large ; 2) The size of graphene glass with uniform quality is limited (diagonal length is less than 4 inches), because the atmospheric pressure CVD growth method limits the macroscopic uniformity of graphene in principle, thereby limiting the graphene glass with uniform quality size of
The deficiencies in these two aspects have seriously affected the future industrial application of graphene glass

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Ultrasonic cleaning is used to place 60cm*6cm (diagonal length about 25 inches) of quartz glass in acetone, ethanol, and deionized water for 10 minutes, blow dry with nitrogen, clean it, and put it into a high-temperature tube at 1100°C. In the type furnace, use an oil-free scroll vacuum pump to pump the pressure in the reaction chamber to below 10Pa, evacuate, and pass Ar / H 2 1000 / 1000sccm, open the ethanol gas valve after the airflow is stable, ethanol vapor enters the reaction chamber and quickly cracks into activated carbon species, a large number of activated carbon species are adsorbed to the surface of quartz glass, migrate and collide on the surface, thereby realizing the nucleation and growth of graphene . The ethanol flow rate was set to 500 sccm, the partial pressure was 250 Pa, and the graphene growth process was set to 4 minutes. After the growth, the ethanol valve was quickly closed, and the Ar / H 2 Set to 300 / 300sccm, start the cooling process of the sam...

Embodiment 2

[0036] Ultrasonic cleaning method is used to place 50cm*6cm quartz glass in acetone, ethanol, and deionized water for 10 minutes, blow dry with nitrogen, clean it, and put it into a 3-inch diameter high-temperature tube furnace at 1100 °C. Use an oil-free scroll vacuum pump to evacuate the pressure in the reaction chamber to below 10Pa, and inject Ar / H 2 1000 / 1000sccm, open the ethanol gas valve after the airflow is stable, ethanol vapor enters the reaction chamber and quickly cracks into activated carbon species, a large number of activated carbon species are adsorbed to the surface of quartz glass, migrate and collide on the surface, thereby realizing the nucleation and growth of graphene . The ethanol flow rate was set to 500 sccm, the partial pressure was 250 Pa, the graphene growth process was set to 10 minutes, and the ethanol valve was quickly closed after the growth was over, and the Ar / H 2 Set to 300 / 300sccm to start the cooling process. After the temperature in th...

Embodiment 3

[0039] Use ultrasonic cleaning method to place 40cm*6cm quartz glass in acetone, ethanol, and deionized water for 10 minutes, blow dry with nitrogen, clean it, put it in a high-temperature tube furnace at 1100°C, and use an oil-free vortex The vacuum pump pumps the pressure in the reaction chamber to below 10Pa, and the Ar / H 2 1000 / 1000sccm, open the ethanol gas valve after the airflow is stable, ethanol vapor enters the reaction chamber and quickly cracks into activated carbon species, a large number of activated carbon species are adsorbed to the surface of quartz glass, migrate and collide on the surface, thereby realizing the nucleation and growth of graphene . The ethanol flow rate was set to 500 sccm, the partial pressure was 250 Pa, the graphene growth process was set to 20 minutes, and the ethanol valve was quickly closed after the growth was over, and the Ar / H 2 Set to 300 / 300sccm to start the cooling process. After the temperature in the reaction chamber drops to ...

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Abstract

The invention discloses a rapid growth method of large-sized graphene glass. The method comprises the following steps that 1) large-sized quartz glass is cleaned; 2) the cleaned quartz glass is placedinto a high-temperature tube furnace, wherein the temperature in a reaction cavity is 1000-1100 DEG C, and the reaction cavity is vacuumized and air is evacuated until the vacuum degree is 10 Pa or below; 3) Ar and H2 are led into the reaction cavity, ethyl alcohol steam is led into the reaction cavity after airflow is stable, and then a graphene growth process is started, wherein the growth timeis 4-30 minutes; and 4) after growth of graphene is completed, the ethyl alcohol steam is cut off, the Ar and H2 flow rate is decreased, Ar / H2 is cut off after the temperature is decreased to the room temperature, and then the large-sized graphene glass is obtained. According to the rapid growth method provided by the invention, the preparation time of the graphene glass is shortened to be 4-30 minutes from a few hours, and by adopting the rapid growth method, graphene glass of a larger size can be prepared.

Description

technical field [0001] The invention belongs to the field of functional materials. Specifically, the invention relates to a kind of use of ethanol as a carbon precursor, and through low-pressure chemical vapor deposition (CVD), a film of graphene with different layer thickness and large size is rapidly grown on the surface of quartz glass, thereby Techniques for obtaining high-quality graphene glass. Background technique [0002] Graphene glass is a new high-performance composite material formed by combining traditional glass materials with graphene. Covering the glass surface with graphene, while maintaining the original good transparency of the glass, endows the glass with the good electrical conductivity, thermal conductivity, surface hydrophobicity and biocompatibility of graphene. An important way to apply orientation. Due to the low cost of glass, it is widely used in daily life, such as smart windows, transparent heating sheets, self-cleaning glass, biological cell ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/44C23C16/26C01B32/182
Inventor 刘忠范陈旭东张艳锋
Owner 北京石墨烯研究院有限公司
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