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Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique

A graphene, ultra-thin technology, applied in gaseous chemical plating, metal material coating process, coating and other directions, can solve problems such as unfavorable energy saving and environmental protection, small output size, generation of exhaust gas, etc., to reduce energy and resource consumption , the shape and size requirements are small, the effect of good industrial prospects

Active Publication Date: 2013-08-28
YICHANG HOUHUANG VACUUM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the methods for preparing graphene mainly include (1) solid-phase method: such as mechanical exfoliation method. (2) Liquid-phase methods: such as redox method, ultrasonic dispersion method, etc., but the graphene prepared by this method also has disadvantages such as low crystallization degree or difficulty in purification and transfer; (3) Chemical vapor deposition method: such as chemical vapor deposition method combined with dissolution-precipitation method (CVD), this method has great advantages in the preparation of single-layer graphene, but there is only a small amount of carbon dissolved by CVD method after quenching. Part of it is analyzed to form graphene, the thickness is not easy to control, and the CVD method requires a high temperature above 1000 ° C and generates waste gas, which is not conducive to energy saving and environmental protection; in addition, ion implantation combined with heat treatment-cooling precipitation method is also a relatively effective method for preparing graphene. method

Method used

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  • Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique
  • Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique
  • Method for preparing graphene or ultrathin carbon film by PVD (physical vapor deposition) technique

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The preparation process in this example is as follows: first, the substrate is placed on the substrate holder in the deposition chamber, and the substrate surface Perform glow cleaning for 20 minutes; then, under the conditions of argon environment and substrate bias -200V, a mixed gas of acetylene and argon is introduced into the deposition chamber, the pressure is 0.55 Pa, the flow rate of acetylene in the mixed gas is 10 sccm, and the argon The flow rate of the gas is 70sccm; the ion source of the anode layer is turned on to ionize the mixed gas, the voltage is 450V during the ionization, the ion source of the anode layer generates a stable ionization current of 1.4A, and the acetylene is ionized to produce carbon-containing cations, and the cations are in the Under the action of an electric field, the substrate is bombarded and deposited on the substrate. The deposition time is 10 minutes. During the deposition process, the substrate rotates with the substrate holder...

Embodiment 2

[0030]The preparation process in this example is as follows: first, the substrate is placed on the substrate holder in the deposition chamber, under the conditions of 90°C, argon atmosphere, vacuum degree of 2.5Pa, and substrate bias of -800V, the surface of the substrate is Perform glow cleaning for 20 minutes; after the glow cleaning of the substrate surface is completed, open the multi-arc target under the conditions of argon atmosphere, substrate bias voltage -100V, and vacuum degree of 0.7 Pa. The target material is high-purity metal copper. The voltage on the metal target is 20V, the current is 40A, the metal is deposited on the surface of the substrate to form a metal catalyst layer, the deposition time is 10min, and the copper metal target is turned off. Then, under the conditions of argon environment and substrate bias-200V, a mixed gas of acetylene and argon is introduced into the deposition chamber, the air pressure is 0.8 Pa, the flow rate of acetylene in the mixed ...

Embodiment 3

[0032] The preparation process in this example is as follows: firstly, the substrate is placed on the substrate holder in the deposition chamber, and the substrate surface Perform glow cleaning for 20 minutes; after the glow cleaning of the substrate surface is completed, open the multi-arc target under the conditions of argon environment, substrate bias voltage -200V, and vacuum degree of 0.5 Pa. The target material is high-purity nickel metal. The voltage on the metal target is 20V, the current is 100A, the metal is deposited on the surface of the substrate to form a metal catalyst layer, the deposition time is 10min, and the copper metal target is turned off. Then, under the condition of argon environment and substrate bias voltage -200V, a mixed gas of acetylene and argon is introduced into the deposition chamber, the pressure is 0.6Pa, the flow rate of acetylene in the mixed gas is 20 sccm, and the flow rate of argon gas is 60 sccm; Turn on the ion source of the anode lay...

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Abstract

The invention provides a method for preparing a graphene or ultrathin carbon film by a PVD (physical vapor deposition) technique, which comprises the following steps: putting a substrate on a substrate rack in a deposition chamber, and carrying out glow cleaning on the substrate surface; introducing an acetylene-argon gas mixture into the gas mixture at 70-100 DEG C in an argon environment under the conditions of vacuum degree 0.5-1 Pa and the substrate voltage bias -200V; opening an anode layer ion source to ionize the gas mixture, wherein the voltage of the anode layer ion source is 300-500V in the ionization process, the acetylene is ionized to generate carbonous cations, and the cations bombards the substrate under the action of an electric field and deposits on the substrate; and after the deposition is finished, annealing under vacuum conditions for 1-2 hours, thereby preparing the graphene or ultrathin carbon film on the substrate surface after the annealing is finished. The method provided by the invention can satisfy the large-scale preparation of uniform-thickness graphene or ultrathin carbon films, and has important industrial application prospects.

Description

technical field [0001] The invention relates to a method for preparing graphene or ultra-thin carbon film by PVD technology, belonging to the technical field of film materials. Background technique [0002] Carbon is an element widely distributed in nature and exists in various forms, such as graphite, amorphous carbon and diamond, as well as carbon nanotubes and graphene discovered in recent years. The properties of different forms of carbon vary greatly, but the reason is that carbon can form several stable hybrid forms, that is, sp 1 hybridization, sp 2 hybridization and sp 3 hybridization. Graphene refers to a single-layer graphite sheet, only one atom thick, composed of sp 2 A honeycomb crystal structure formed by the close arrangement of hybridized carbon atoms. The carbon-carbon bond length in graphene is about 0.142nm. There are three σ bonds in each lattice, which are very firmly connected, forming a stable hexagonal shape. Visually speaking, graphene is a tw...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C23C16/26C23C16/50
Inventor 闫少建林宝珠付德君
Owner YICHANG HOUHUANG VACUUM TECH
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