Method for efficiently eliminating graphene wrinkles formed by chemical vapor deposition

Patent metadata

Field	Value
Publication number	US-12116281-B2
Application number	US-201917416525-A
Country	US
Kind code	B2
Filing date	Dec 24, 2019
Priority date	Feb 20, 2019
Publication date	Oct 15, 2024
Grant date	Oct 15, 2024

Abstract

A method for efficiently eliminating graphene wrinkles formed by chemical vapor deposition includes: directly growing super smooth wrinkle-free graphene films on metal substrates such as copper, nickel and alloys thereof and non-metal substrates such as silicon oxide and silicon carbide, or eliminating the wrinkles of wrinkled graphene through controlled proton injection at a high temperature by precisely controlling the temperature and hydrogen plasma power and time for generating protons; where the plasma-assisted chemical vapor deposition system includes a plasma generator, a vacuum system and a heating system; where the power of the plasma generator is 5 to 1000 W, the pressure of the vacuum system is 10−5 to 105 Pa, and the heating temperature of the system is controllable between 25 to 1000° C.; directly growing a super smooth wrinkle-free graphene by injecting protons on various substrates during growth.

First claim

What is claimed is:

1. A method for eliminating graphene wrinkles formed by chemical vapor deposition, comprising steps of treating a wrinkled graphene to reduce and eliminate the wrinkles:
step 1: placing the wrinkled graphene formed on metal substrates or non-metal substrates by a conventional chemical vapor deposition in a plasma-assisted chemical vapor deposition system, heating at a specific hydrogen pressure for a certain time, and adjusting an appropriate coupled matching power and reaction time for plasma reaction to reduce and eliminate the graphene wrinkles; and adjusting, by the plasma-assisted chemical vapor deposition technology, the reaction temperature, pressure, reaction gas flow, heating time, plasma intensity and reaction time; wherein the reaction temperature is 100 to 1000° C., the reaction pressure is 1 to 100 Pa, the reaction gas includes hydrogen, the gas flow is 5 to 2000 sccm, the heating time is 60 to 3600 s, and the plasma reaction time is 60 to 1800 s.

2. The method according to claim 1 , wherein the wrinkled graphene is prepared by chemical vapor deposition, and a wrinkled graphene film is grown by adjusting the reaction temperature, pressure and carrier gas flow; wherein the reaction temperature is 600 to 1400° C., the pressure is 10 −2 to 10 5 Pa, a carbon source gas includes methane, ethylene, acetylene and various carbon-containing organic substances which are gaseous, liquid or solid, the gas flow is 10 −5 to 100 sccm, a carrier gas is hydrogen, nitrogen, helium, or argon, the gas flow is generally 5 to 5000 sccm, and the reaction time is 5 to 3600 s.

3. The method according to claim 1 , wherein for the subsequent treatment of the wrinkled graphene, the heating time is 60 to 3600 s, and the heating temperature is 100 to 1000° C.; the plasma power is 10 to 500 W, the plasma reaction time is 1 to 30 min, and the reaction pressure is 1 to 100 Pa.

4. The method according to claim 1 , wherein the metal substrates comprises copper, nickel, platinum, iridium, ruthenium, tungsten, gold or silver, and the non-metal substrates comprises silicon oxide, aluminum oxide or silicon carbide.

5. The method according to claim 1 , wherein a plasma generator used in the plasma-assisted chemical vapor deposition technology is an inductively coupled RF plasma with the power adjustable from 5 to 1000 W, the pressure of the vacuum system is adjustable from 10 −5 to 10 5 Pa, and the temperature of the heating system is controllable between 25 to 1000° C.

6. The method according to claim 1 , wherein the height of the wrinkles is reduced or eliminated, and is less than or equal to 3 nm for single-layer graphene.

Assignees

• Nanjing University

Inventors

• Gao Libo
• Yuan Guowen
• Xu Jie

Classifications

• H01J2237/3321

  CVD [Chemical Vapor Deposition] · CPC title

• H01J37/32816

  Pressure · CPC title

• H01J37/321

  the radio frequency energy being inductively coupled to the plasma · CPC title

• C23C16/52

  Controlling or regulating the coating process {(C23C16/45557, C23C16/279 take precedence)} · CPC title

• C23C16/50

  using electric discharges {(generation and control of plasma in discharge tubes for surface treatment H01J37/32, H01J37/34)} · CPC title