A method of growing multilayer graphene on copper-iron alloys

Abstract

The application discloses a method for growing multilayer graphene on copper-iron alloy, comprising the following steps: S1, placing Cu x Fe 100‑x (70≤x<100) alloy in a tube furnace, annealing for 30-60 minutes under argon-hydrogen mixed gas at 900-1000 DEG C under normal pressure; S2, after annealing, introducing carbon-containing gas, and heat preserving for 5-120 minutes; S3, closing the carbon-containing gas, and reducing the temperature to 600 DEG C under argon-hydrogen mixed gas atmosphere; S4, closing the hydrogen, and rapidly reducing the temperature to room temperature under argon atmosphere, and taking out the sample. The method for growing multilayer graphene on copper-iron alloy is simple and easy to operate, and has high yield.

Description

Technical Field

[0001] This invention belongs to the field of advanced materials technology and relates to a method for growing multilayer graphene on copper-iron alloy. The method effectively grows multilayer continuous graphene films on copper-iron alloy, is simple and easy to implement, has a high yield, and the cost of copper-iron alloy is lower than that of pure copper foil, making it suitable for large-scale production. Background Technology

[0002] Graphene is composed of sp 2 Graphene, a two-dimensional inorganic crystalline material composed of hybrid carbon atoms in a hexagonal honeycomb structure, has only one carbon atom layer and a thickness of only 0.335 nm. The discovery of graphene has caused a huge stir in the scientific community, and its emergence is expected to trigger a new revolution in the field of new materials. CVD is a convenient and effective method for large-scale preparation of graphene. In some applications, such as heat dissipation, it is necessary to grow multi-layered or even thicker graphene films. Although multi-layered graphene can be grown on nickel foil, the bonding between the nickel foil and graphene is quite strong, making it impossible to transfer graphene from the nickel foil using dry transfer methods. Therefore, the current conventional method is still wet transfer, using chemical reagents to etch away the nickel foil. This method makes it impossible to recycle the nickel foil, resulting in a significant increase in production costs and hindering end-use applications; at the same time, the production process also generates a large amount of chemical waste liquid, impacting environmental pollution. Graphene grown on copper can be transferred using a bubbling method, allowing the copper foil to be reused and saving costs. However, due to the self-limiting effect, it is difficult to grow multi-layered or thicker continuous graphene films on copper foil.

[0003] The method provided by this invention patent can overcome the above difficulties and can grow multilayer graphene continuous films on copper-iron alloys. The method is simple and easy to implement, with a high yield. The cost of copper-iron alloys is lower than that of pure copper foils, making it suitable for large-scale production. Summary of the Invention

[0004] This invention provides a method for growing multilayer graphene on a copper-iron alloy. The method is simple, easy to implement, and has a high yield. The cost of copper-iron alloy is lower than that of pure copper foil, making it suitable for large-scale production.

[0005] The technical solution provided by this invention is as follows: A method for growing multilayer graphene on a copper-iron alloy includes the following steps: S1, Cu x Fe 100-x (70≤x<100) The alloy was placed in a tube furnace and heated to 900-1000℃ under normal pressure in an argon-hydrogen mixture for 30-60 minutes. S2. After annealing, introduce carbon-containing gas and hold at the temperature for 5-120 minutes; S3. Turn off the carbon-containing gas and lower the temperature to 600℃ in an argon-hydrogen mixed atmosphere; S4. Turn off the hydrogen gas and rapidly cool the sample to room temperature under an argon atmosphere. Remove the sample.

[0006] Preferably, in step S1, the copper-iron alloy is selected from Cu. 70 Fe 30 .

[0007] Preferably, the heating rate is controlled to be from 0.1 ℃ / min to 20 ℃ / min.

[0008] Preferably, the cooling rate is controlled to be >20 ℃ / min.

[0009] The present invention can bring the following beneficial effects: 1) This invention enables the growth of multilayer graphene on copper-iron alloys.

[0010] 2) The method of the present invention is simple and easy to implement, with a high yield. The cost of copper-iron alloy is lower than that of pure copper foil, making it suitable for large-scale production. Attached Figure Description

[0011] Figure 1 This is an image of a multilayer graphene film peeled off a copper-iron alloy.

[0012] Figure 2 This is the Raman spectrum of the multilayer graphene film prepared in the example. Detailed Implementation

[0013] To facilitate understanding of this application and to make the aforementioned objectives, features, and advantages of this application more apparent, a detailed description of specific embodiments of this application is provided below in conjunction with the accompanying drawings. Numerous specific details are set forth in the following description to provide a thorough understanding of this application, and preferred embodiments are shown in the accompanying drawings. However, this application can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and complete understanding of the disclosure of this application. This application can be implemented in many other ways different from those described herein, and those skilled in the art can make similar modifications without departing from the spirit of this application; therefore, this application is not limited to the specific embodiments disclosed below.

[0014] To keep the drawings simple, each drawing only schematically shows the parts related to the present invention, and they do not represent the actual structure of the product.

[0015] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of this application.

[0016] A method for growing multilayer graphene on a copper-iron alloy includes the following steps: S1, Cu x Fe 100-x (70≤x<100) The alloy was placed in a tube furnace and heated to 900-1000℃ under normal pressure in an argon-hydrogen mixture for 30-60 minutes. S2. After annealing, introduce carbon-containing gas and hold at the temperature for 5-120 minutes; S3. Turn off the carbon-containing gas and lower the temperature to 600℃ in an argon-hydrogen mixed atmosphere; S4. Turn off the hydrogen gas and rapidly cool the sample to room temperature under an argon atmosphere. Remove the sample.

[0017] Example Specific experiments were conducted based on the above experimental steps, resulting in the following examples: S1, Cu 70 Fe 30 The alloy was placed in a tube furnace, and under normal pressure, 500 sccm of argon and 50 sccm of hydrogen were introduced. The temperature was raised to 900℃ and annealed for 30 minutes. S2. After annealing, introduce 5 sccm of methane and hold at 900℃ for 60 minutes. S3. Turn off methane, and continue to introduce 500 sccm of argon and 50 sccm of hydrogen to lower the temperature to 600℃ at a rate of 25℃ / min. S4. Turn off the hydrogen gas and continue to purge with argon gas at a rate of 500 sccm. Cool the sample to room temperature at a rate of 30℃ / min, then remove the sample (e.g., Figure 1 (As shown).

[0018] S5. Test the sample using Raman spectroscopy.

[0019] The obtained graphene film is intact and has no obvious defects.

[0020] It should be noted that the above description is only a preferred embodiment of the present invention. For those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A method for growing multilayer graphene on a copper-iron alloy, comprising the following steps: S1, Cu x Fe 100-x (70≤x<100) The alloy was placed in a tube furnace and heated to 900-1000℃ under normal pressure in an argon-hydrogen mixture for 30-60 minutes. S2. After annealing, introduce carbon-containing gas and hold at the temperature for 5-120 minutes; S3. Turn off the carbon-containing gas and lower the temperature to 600℃ in an argon-hydrogen mixed atmosphere; S4. Turn off the hydrogen gas and rapidly cool the sample to room temperature under an argon atmosphere. Remove the sample.

2. The method for growing multilayer graphene on a copper-iron alloy according to claim 1, characterized in that: The Fe content should be controlled to ≤30% to avoid excessive carbon dissolution.

3. The method for growing multilayer graphene on the surface of copper foil according to claim 1, characterized in that: After high-temperature annealing, a copper-rich region forms on the surface, achieving self-limited growth similar to pure copper. Carbon dissolved in iron in the bulk phase slowly precipitates through the copper layer upon cooling, promoting the growth of the underlying graphene.

4. The method for growing multilayer graphene on the surface of copper foil according to claim 1, characterized in that: Rapid cooling prevents carbon from precipitating out in the form of Fe3C.

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