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Method for removing carbon deposition on inner wall of air inlet pipe in CVD (Chemical Vapor Deposition) grown graphene powder

A graphene powder and air intake pipe technology, applied in the graphene field, can solve problems such as increased energy consumption, reduced pyrolysis efficiency, and air flow blockage, and achieves the effects of saving production costs, improving service life, and shortening intervals

Pending Publication Date: 2022-04-08
2D CARBON CHANGZHOU TECH INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when graphene powder is grown in molten metal by CVD method, as the growth continues, the long-chain by-products of methane cracking will deposit carbon on the inner wall of the inlet nozzle inserted into the molten metal, causing the inlet pipe The inner diameter of the mouth continues to decrease, which eventually causes the airflow to be blocked, so that it is impossible to continue to aerate and grow graphene powder
[0005] Currently commonly used methods to remove carbon deposits in the intake pipe: the first is to use a drill to drill out the carbon deposits on the inner wall of the intake pipe; The rate of carbon deposition on the wall; at present, there are certain defects in both methods: the first method must stop the growth, the temperature in the high-temperature furnace drops to room temperature, open the furnace cover, and take out the intake pipe to use a drill to drill the inner wall of the intake pipe. Carbon drilling, this method not only has a long interval between graphene growth before and after, but also increases energy consumption after repeated heating and cooling, and the powder growth efficiency is low; while the second method can slow down the speed of carbon deposition on the inner wall of the intake pipe, However, the pyrolysis efficiency of carbon-containing gas will also decrease, which will affect the growth efficiency of graphene powder

Method used

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  • Method for removing carbon deposition on inner wall of air inlet pipe in CVD (Chemical Vapor Deposition) grown graphene powder
  • Method for removing carbon deposition on inner wall of air inlet pipe in CVD (Chemical Vapor Deposition) grown graphene powder

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Embodiment 1

[0033] Embodiment 1: a method for removing carbon deposits on the inner wall of the intake pipe in a CVD-grown graphene powder, comprising the following steps:

[0034] S1. Insert the graphite inlet pipe into the liquid copper through the lifting device, and then pass the mixed gas of methane / nitrogen into the liquid copper through the graphite inlet pipe, grow graphene powder in the liquid copper, and the graphene powder grows continuously for 8- After 12 hours, disconnect the methane, keep the nitrogen flow constant, and suspend the growth of graphene powder;

[0035]S2. By adjusting the heating power, the temperature of the liquid copper is kept at 1100°C to 1600°C, and the preferred temperature of the liquid copper is 1150°C to 1400°C; in this embodiment, the temperature of the lower part of the graphite intake pipe is raised to Within the temperature range where carbon deposits and oxygen can react, ensure that the carbon deposits on the inner wall of the graphite inlet p...

Embodiment 2

[0046] Embodiment 2: the specific implementation steps of this embodiment are as follows:

[0047] 1) Insert the graphite inlet pipe into the liquid copper at 1290°C through the lifting device, and then pass the methane / nitrogen mixed gas into the liquid copper through the graphite inlet pipe. The flow rates of methane and nitrogen are 4SLM / 30SLM respectively, and grow in the liquid copper Graphene powder, grow continuously for 8 hours, cut off methane, and suspend the growth of graphene powder;

[0048] 2) Adjust the heating power so that the temperature of the liquid copper is at 1300°C;

[0049] 3) Move the gas outlet at the lower part of the graphite inlet pipe out of the liquid copper surface by a lifting device at a distance of 2cm; after 1.5min, feed the oxygen / nitrogen mixed gas, wherein the flow rates of oxygen and nitrogen are 2SLM / 20SLM respectively;

[0050] 4) After the oxygen / nitrogen mixed gas is introduced for 2 minutes, the oxygen is disconnected, the nitroge...

Embodiment 3

[0053] Embodiment 3: the specific implementation steps of this embodiment are as follows:

[0054] 1) Insert the graphite inlet pipe into the liquid copper at 1220°C through the lifting device, and then pass the methane / nitrogen mixed gas into the liquid copper through the graphite inlet pipe. The flow rates of methane and nitrogen are 4.5SLM / 30SLM respectively, in the liquid copper Grow graphene powder, grow continuously for 10 hours, cut off methane, and suspend the growth of graphene powder;

[0055] 2) Adjust the heating power so that the temperature of the liquid copper is at 1250°C;

[0056] 3) Move the gas outlet at the lower part of the graphite inlet pipe out of the liquid copper surface by a lifting device at a distance of 4cm; after 50s, feed oxygen / nitrogen mixed gas, wherein the flow rates of oxygen and nitrogen are 3SLM / 20SLM respectively;

[0057] 4) After the oxygen / nitrogen mixed gas is introduced for 1 minute, the oxygen is disconnected, the nitrogen flow ra...

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Abstract

The invention discloses a method for removing carbon deposition on the inner wall of a gas inlet pipe in CVD (Chemical Vapor Deposition) grown graphene powder, which comprises the following steps: S1, inserting a graphite gas inlet pipe into liquid metal, then introducing mixed gas containing carbon source gas / nitrogen into the liquid metal through the graphite gas inlet pipe, and growing graphene powder in the liquid metal, after the graphene powder continuously grows for a preset time, cutting off the carbon source-containing gas, keeping the nitrogen flow unchanged, and suspending the growth of the graphene powder; s2, the temperature of the molten liquid metal is adjusted; s3, a gas outlet of the graphite gas inlet pipe is moved out of the liquid level of the liquid metal, and then oxygen / nitrogen mixed gas is introduced into the graphite gas inlet pipe; and S4, after the oxygen / nitrogen mixed gas is introduced for a set time, the oxygen is cut off, the nitrogen is kept unchanged, and cooling is conducted. According to the method, carbon deposition on the inner wall of the air inlet pipe can be efficiently removed, operation is easy, the interval time from pausing of growth of the graphene powder to re-growth is short, and the growth efficiency of the graphene powder is high.

Description

technical field [0001] The invention belongs to the technical field of graphene, and in particular relates to a method for removing carbon deposits on the inner wall of an intake pipe in a CVD-grown graphene powder. Background technique [0002] Graphene is a two-dimensional honeycomb crystal material composed of carbon atoms hybridized with SP2. Due to its excellent optical, electrical, and mechanical properties, it has important application prospects in the fields of materials science, micro-nano processing, energy, and biomedicine, so it has attracted extensive attention from many researchers. [0003] At present, the preparation methods of graphene powder include mechanical exfoliation method, redox method and CVD (chemical vapor deposition) method; although mechanical exfoliation method can prepare graphene powder with few defects, the number of graphene layers is thick and the preparation cost is high ; Although the redox method can prepare graphene powder at a lower ...

Claims

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Application Information

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IPC IPC(8): B08B9/032C01B32/186
Inventor 王增奎金虎邓科文常博文
Owner 2D CARBON CHANGZHOU TECH INC
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