阅读说明：本技术 真空舱隧道炉、管式线性供气生产大面积石墨烯单晶膜 (Vacuum chamber tunnel furnace and tubular linear gas supply production large-area graphene single crystal film ) 是由 汪又翔 于 2018-06-29 设计创作，主要内容包括：本发明是在真空舱中设置隧道炉、铜镍箔移动装置；在隧道炉中设置点式和管式线性供气装置,铜镍箔移动装置移动铜镍箔与沉积气体反应裂解生产单晶石墨烯薄膜,属于化学气相沉积法。本发明解决了现在气相沉积法沉积气体自由散落生产多晶畴石墨烯膜的缺陷问题,同时克服了单晶石墨烯无法量产的问题。点式供气装置供气有效控制单晶石墨烯初步形成,管式线性供气装置逐步扩大单晶石墨烯薄膜横向面积,稳定后的管式线性供气装置供气保证了大面积单晶石墨烯连续生产的需要,这样使大面积的单晶石墨烯薄膜达到大批量生产。(The invention is that a tunnel furnace and a copper-nickel foil moving device are arranged in a vacuum chamber; a point-type and tubular linear gas supply device is arranged in a tunnel furnace, a copper-nickel foil moving device moves a copper-nickel foil to react with deposition gas for cracking to produce a single crystal graphene film, and the method belongs to a chemical vapor deposition method. The method solves the defect that the existing vapor deposition method can produce the multi-domain graphene film by freely scattering the deposited gas, and simultaneously solves the problem that the single crystal graphene can not be produced in large quantity. Point type air feeder air feed effective control single crystal graphene is preliminary formed, and the horizontal area of single crystal graphene film is progressively enlarged to the linear air feeder of tubular, and the linear air feeder air feed of tubular after the stability has guaranteed the needs of large tracts of land single crystal graphene continuous production, makes the single crystal graphene film of large tracts of land reach mass production like this.)

1. The production process comprises the steps of centralized gas supply of a point type and tubular type linear gas supply device, movement of a copper-nickel foil moving device, large-area continuous mass production of graphene single crystal films under the protection of argon and the like.

2. Tunnel furnaces, point and tubular linear gas supply devices and copper-nickel foil moving devices in vacuum chambers are necessary practical devices for producing large-area single-crystal graphene films.

The technical field is as follows:

the invention relates to the field of graphene preparation and production. Methods of preparing graphene are roughly divided into physical preparation methods and chemical preparation methods. The invention belongs to a chemical preparation method, and discloses a method for realizing large-scale production of a large-area single-crystal graphene film by a vapor deposition method (CVD) through point-type and tubular linear gas supply by applying a tunnel furnace in a vacuum chamber.

Background art:

at present, both graphene powder materials and single-layer graphene films can be produced in large scale. However, a single-layer graphene film produced by a vapor deposition method is a polycrystalline film, and the electrical, mechanical, thermal and optical properties of the graphene film are seriously damaged by grain boundary defects formed by splicing of polycrystalline crystal domains. Although many scientists in various countries strive, the meter-scale single crystal graphene film is still not prepared, and more particularly, the large-scale mass production is realized.

The invention content is as follows:

the point-mode and tubular linear gas supply of the tunnel furnace in the vacuum chamber is a better method for producing the large-area graphene single crystal film. The method is that a tunnel furnace is arranged in a vacuum chamber, an electric heating device is arranged at the bottom in the furnace, a copper-nickel foil moving device moves the copper-nickel foil to a preset temperature, and a group of point type and a plurality of groups of tubular linear gas supply devices (arranged at fixed positions) are arranged. The tubular linear air supply device is characterized in that air supply ports are arranged in a line. The diameter of the air outlet of the point type air supply device is 0.1 mm. The point type air supply device and the tubular linear air supply device are arranged in a triangle. Firstly, point type air supply devices are arranged, and tubular linear air supply devices are arranged according to the length of 0.1m to 1 m. (the gas supply device is close to the copper nickel foil and is 1-2mm away from the copper nickel foil).

Firstly, supplying gas by a point type gas supply device, opening a first group of tubular linear gas supply devices for supplying gas when the preset time is up, and closing the point type gas supply devices; and similarly, opening the second group of tubular linear gas supply devices for supplying gas according to the preset time, and closing the first group of tubular linear gas supply devices at the same time, so that the last group of tubular linear gas supply devices with the length of 1m are opened for supplying gas (other gas supply devices are all closed), and stopping supplying gas until the copper-nickel foil is moved. The deposited gas is close to the moved copper-nickel foil for reaction and cracking, and the defect that the deposited gas freely scatters the multi-domain graphene film is overcome.

The arrangement of the vacuum chamber ensures that useful gas enters the tunnel furnace and raw materials and products can continuously and quickly enter and exit; the arrangement of the tunnel furnace ensures the temperature requirements of each section of the copper-nickel foil cracking deposition gas, and the yield can be improved by improving the length (namely the complete reaction time is completed in the subsequent space); the arrangement of the copper-nickel foil moving device ensures that the copper-nickel foil can meet the requirement of the reaction cracking of the deposited gas; the arrangement of the point type and tubular linear gas supply device ensures the controllable formation of the single crystal graphene film and the gas requirement of each section. Therefore, a complete single-crystal graphene film mass production line is formed from the steps of raw material and product inlet and outlet, other inhibited gas inlet, deposited gas reaction cracking, copper-nickel foil heating reaction cracking to single-crystal graphene film output.

The specific implementation mode is as follows:

firstly, the copper-nickel foil is installed and then vacuumized. Pumping out all air which is not beneficial to production in the vacuum chamber tunnel furnace, and injecting H, Ar gas (H, Ar is 5: 1) into the vacuum chamber and the tunnel furnace to reach normal pressure (H controls CH)₄When the gas rises, Ar ensures that CH is not participated₄The cracked copper nickel foil is not contaminated), i.e. the gas supply is stopped.

And secondly, heating the tunnel furnace, keeping 800 ℃ in the furnace, and supplying gas according to the opening and closing procedures of the point type and tubular type linear gas supply devices when the temperature of the copper nickel foil under the point type and tubular type linear gas supply devices is 1000 ℃ after each section of the furnace meets the requirements. Opening point type gas supply and starting the copper-nickel foil moving device at the same time; CH (CH)₄The amount of Ar supplied was changed with the point type gas supply device and the tubular linear gas supply device. Normal posterior CH₄The air supply amount per minute is 1ml, and Ar is determined according to the actual use amount of the vacuum chamber and the tunnel furnace. The moving speed of the copper-nickel foil is 2 cm/s. The length of each roll of the copper-nickel foil is 480 m.

Thirdly, after the copper nickel foil is moved, closing CH₄Ar is used for air supply, and then the roll is automatically changed. And when the temperature of the copper nickel foil at the point-type and tubular linear gas supply device reaches 1000 ℃, simultaneously starting the gas supply and copper nickel foil moving devices according to the program (the gas supply is stopped when automatic roll changing equipment is not arranged, all the gas in the vacuum cabin and the tunnel furnace is pumped into a waste gas storage tank, and the gas is separated and then used). Normal air is injected (without stopping heat supply), the cabin door is opened, the coil is changed, the product is moved out, and the equipment condition is checked. After the completion, the cabin door is closed, and then the vacuum pumping is carried out to repeat the working procedure.