CN112429724A

CN112429724A - Preparation method of five-layer graphene

Info

Publication number: CN112429724A
Application number: CN202011617800.XA
Authority: CN
Inventors: 郝玉峰; 陆洪彬; 唐伟
Original assignee: Nantong Jingrui New Carbon Material Technology Co ltd
Current assignee: Nantong Jingrui New Carbon Material Technology Co ltd
Priority date: 2020-12-31
Filing date: 2020-12-31
Publication date: 2021-03-02

Abstract

The invention discloses a preparation method of five-layer graphene, which is prepared by a chemical vapor deposition system, wherein a cobalt-nickel alloy foil is used as a growth substrate to grow large-area four-six-layer graphene, and the average thickness of the graphene is five layers; the metal foil substrate is arranged in the center of the inner part of the quartz tube, and the quartz tube is arranged in the resistance wire tube furnace; the gas source for growing the five-layer graphene is methane, ethylene or acetylene and hydrogen, and the growth temperature is 900-; the growth time is 30-600 minutes; the system pressure ranges from 0.1Torr to atmospheric pressure.

Description

Preparation method of five-layer graphene

Technical Field

The invention relates to a preparation method of a graphene material, in particular to a preparation method of five-layer graphene.

Background

Graphene is an SP2 hybridized monoatomic layer carbon material with the room-temperature carrier fluid mobility of more than 10,000cm²V^-1s^-1And the mobility of silicon is two orders of magnitude higher than that of silicon in a traditional microelectronic circuit, so that graphene may play an important role in future electronic devices. However, graphene is a semimetal with zero band gap, which means that a graphene electronic device cannot realize a complete off state, which is an intrinsic defect of graphene in the field of electronics, and cannot be solved at present. In addition, graphene has a limited mechanical strength and is susceptible to breakage during processing.

The difference between the structure of multi-layer graphene (such as five-layer graphene) with AB stacking and that of single-layer graphene is 4 layers of carbon atoms, and experiments show that the mechanical strength of the five-layer graphene is greatly higher than that of a single layer, and the conductivity of the five-layer graphene is several times higher than that of the single layer, so that the five-layer graphene has a very bright prospect in many fields such as mechanical sensors, transparent conductive films and the like. The preparation of multilayer graphene such as five layers is a hot problem for research and application.

Disclosure of Invention

The invention aims to grow large-area four-six-layer graphene by using a chemical vapor deposition system as growth equipment and using a cobalt-nickel alloy foil as a growth substrate, wherein the average thickness of the graphene is five layers.

The technical scheme of the invention is that a chemical vapor deposition system is used as a growth preparation system, and a cobalt-nickel alloy foil is used as a growth substrate to grow large-area five-layer graphene; the metal foil substrate is placed in a quartz tube and other confined spaces, and five layers of graphene can grow on the same metal foil substrate (such as cobalt-nickel alloy foil) through vapor deposition; the gas source for growing the graphene is methane, ethylene or acetylene and hydrogen, and the growth temperature is 900-; the growth time is 30-600 minutes; the system pressure ranges from 0.1Torr to atmospheric pressure.

The metal foil is positioned in the center of the quartz tube, and the whole quartz tube is placed in the tube furnace.

The system pressure ranges from 0.1Torr to atmospheric pressure (the pressure within the growth system is regulated by argon).

The metal foil growth substrate can also be placed above a metal foil made of another metal foil, and five layers of graphene can be deposited on the cobalt-nickel foil of the growth substrate through vapor deposition; as shown in the following figures.

Has the advantages that: the invention takes a chemical vapor deposition system as growth equipment, and metal foil as a growth substrate to grow large-area four-six-layer graphene, wherein the average thickness of the graphene is five layers. The five layers of graphene grown on the metal foil can be used as a pressure-sensitive material of a mechanical sensor, so that a high-performance sensing device is realized.

Drawings

FIG. 1 is a diagram of an apparatus of the present invention.

Fig. 2 is a four-six layer graphene with an average thickness of five layers on a metal foil substrate.

Detailed Description

FIG. 1 shows an experimental setup according to the present invention, which is a tube furnace, in which a quartz tube with an inner diameter of about 2 inches is placed and a Co-Ni alloy foil is placed at the center inside the quartz tube, and the heating element of the tube furnace is a resistance wire and the heating temperature can reach 1100 ℃.

Growing five layers of graphene on the surface of the cobalt-nickel metal foil substrate through chemical vapor deposition; the gas source for growing the graphene is methane (the methane can be replaced by ethylene or acetylene) and hydrogen, and the growth temperature is 900-; the growth time is 30-600 minutes; the system pressure ranges from 0.1Torr to atmospheric pressure. It is emphasized here that the five-layer graphene obtained using cobalt-nickel alloy foils is similar in characteristics, with a thickness in the range of four to six layers.

The size of the metal foil substrate is only determined by the size of the growth system, i.e. a small system can only accommodate a small growth substrate, and a large system space can accommodate a large size growth substrate.

More specific growth conditions: the gas source of the growth gas is methane and hydrogen, and the growth temperature is about 900-; the growth time is 30-600 minutes; the system pressure is about 0.1Torr to atmospheric pressure. The flow volume ratio of the methane to the hydrogen is 0.1:1-100: 1; the surface of the cobalt-nickel alloy foil in the pocket and the tube can grow five layers of graphene with large area.

The pressure in the growth system was also regulated by argon gas.

The thickness of the cobalt-nickel metal foil is 25-100 microns, and the purity is 99.8%; copper-nickel alloys and the like have similar effects; namely, can grow; but require other parameters to cooperate. The thickness range of the metal foil for manufacturing the metal foil pocket is 25 micrometers to 100 micrometers;

growth system pressure 0.1Torr, higher or lower pressures are similarly effective, but other parameters are required to cooperate;

the growth temperature is 900-; the growth time is 30-600 minutes;

the gas source is hydrogen and methane, argon is used for regulating and controlling the overall pressure of the system, the hydrogen flow is 0-500 standard cubic centimeters per minute (s.c.c.m), and the methane flow is 0-100 s.c.c.m.

The average size of the five-layer graphene film is larger than 1 cm, the thickness range of the five-layer graphene film is four-six-layer graphene, and the average thickness of the five-layer graphene film is five layers.

Five layers of graphene can be deposited on a growth substrate metal foil by vapor deposition; the growth conditions of the photographs of the five-layer graphene on the metal foil substrate were obtained according to the specific parameters of the examples.

Claims

1. The preparation method of the five-layer graphene is characterized in that a chemical vapor deposition system is used as a growth preparation system, a cobalt-nickel alloy foil is used as a growth substrate to grow four-six-layer graphene with large area, and the average thickness of the four-six-layer graphene is five layers; the metal foil substrate is placed in the center of the inner part of the quartz tube, the quartz tube is placed in the resistance wire tube furnace, and five layers of graphene can grow on the metal foil substrate through vapor deposition; the gas source for growing the graphene is methane, ethylene or acetylene and hydrogen, and the growth temperature is 900-; the growth time is 30-600 minutes; the system pressure ranges from 0.1Torr to atmospheric pressure.

2. The method for preparing five-layer graphene according to claim 1, wherein the metal foil is placed in the center of a quartz tube, and the quartz tube is placed in a resistance wire tube furnace.

3. The method for preparing five-layer graphene according to claim 1 or 2, wherein the metal foil is made of cobalt-nickel alloy, and the cobalt-nickel alloy foil is placed in the center of the quartz tube.

4. The method for preparing five-layer graphene according to claim 1 or 3, wherein the flow volume ratio of methane to hydrogen is 0.1:10 to 10: 1000.

5. The method of preparing five-layer graphene according to claim 1 or 3, wherein the pressure in the growth system is controlled by argon gas.

6. The method for preparing five-layer graphene according to claim 1 or 3, wherein the substrate is a cobalt-nickel alloy foil.