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Preparation method of blue and purple fluorescent single-layer N-doped graphene

A technology of nitrogen-doped graphene and fluorescence, which is applied in the direction of single-layer graphene, graphene, chemical instruments and methods, etc., to achieve simple operation and good repeatability

Inactive Publication Date: 2018-10-02
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And by adopting the chemical vapor deposition method to carry out the preparation of graphene, and carry out the relevant research of fluorescence luminescence, there is no report

Method used

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  • Preparation method of blue and purple fluorescent single-layer N-doped graphene
  • Preparation method of blue and purple fluorescent single-layer N-doped graphene
  • Preparation method of blue and purple fluorescent single-layer N-doped graphene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The device used in this example is the BTF-1200C-S-SSL-PECVD tube furnace produced by Anhui Beiike Equipment Technology Co., Ltd. The quartz tube has an outer diameter of 50 mm and an inner diameter of 44 mm.

[0021] (1) 0.01g (calculated according to the volume of the tube furnace, is 0.87g / m 3 ) Melamine is placed in a heating zone in front of the tube furnace, copper foil is placed in a heating zone behind the tube furnace, and then the temperature rise program is set. First, 500 sccm of argon gas is introduced for about 20 minutes to exhaust the air in the tube furnace, and then Under the conditions of 300sccm argon and 100sccm hydrogen, the temperature was raised to 1030°C and kept for 30 minutes to etch the oxide on the surface of the copper foil to prevent it from affecting the contact between the gas carbon source and the copper foil, and then the temperature dropped to 900°C.

[0022] (2) The first temperature zone is raised to 350° C., and at this moment, me...

Embodiment 2

[0025] (1) Place 0.1g of melamine in a heating zone in front of the tube furnace, put the copper foil in a heating zone behind the tube furnace, and then set the temperature rise program. The air is exhausted, and then the temperature is raised to 1030°C under the conditions of 300sccm argon and 100sccm hydrogen, and it is maintained for 30 minutes. The purpose is to etch the oxide on the surface of the copper foil to prevent it from affecting the contact between the gas carbon source and the copper foil. to 1000°C.

[0026] (2) The first temperature zone is raised to 350° C., and at this moment, methane gas is fed in at a gas flow rate of 1 sccm, argon gas at 1000 sccm, and hydrogen gas at 20 sccm. Keep this temperature for 20 minutes, and then under the condition of argon gas flow rate of 300 sccm, the copper foil is rapidly lowered to room temperature to obtain a large-area graphene film.

[0027] The Raman pattern of the sample in this embodiment is as follows figure 2 ...

Embodiment 3

[0029] (1) Place 0.05g of melamine in a heating zone in front of the tube furnace, put the copper foil in a heating zone behind the tube furnace, and then set the temperature rise program, first pass in 500 sccm of argon for about 20 minutes The air is exhausted, and then the temperature is raised to 1030°C under the conditions of 300 sccm argon and 100 sccm hydrogen, and it is kept for 30 minutes. to 950°C.

[0030] (2) The first temperature zone is raised to 350° C., and at this moment, methane gas is fed in at a gas flow rate of 1 sccm, argon gas at 1000 sccm, and hydrogen gas at 20 sccm. Keep this temperature for 20 minutes, and then under the condition of argon gas flow rate of 300 sccm, the copper foil is rapidly lowered to room temperature to obtain a large-area graphene film.

[0031] The fluorescence spectrogram of sample in this embodiment is as follows image 3 As shown in (2), it can be seen from the figure that compared with Example 1 ((1) in the figure), the fl...

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Abstract

The invention relates to a preparation method of blue and purple fluorescent single-layer N-doped graphene. The preparation method comprises steps as follows: a single quartz tube is adopted to cooperate with a tube furnace, and a certain mass of melamine is put in a first temperature zone of the tube furnace; a copper substrate is put in a second temperature zone of the tube furnace; the second temperature zone is heated under the argon and hydrogen atmosphere, and the copper substrate is subjected to annealing treatment; under the argon and hydrogen atmosphere, the copper substrate is reduced to the reaction temperature, and melamine is heated to sublimation temperature; mixed gas of hydrogen, methane and argon is introduced; the copper substrate is reduced to the room temperature, and an N-doped graphene material is obtained. With the adoption of the method, a larger-area N-doped graphene film which is uniform in film forming can be obtained.

Description

technical field [0001] The invention relates to a preparation method of two-dimensional nitrogen-doped graphene, which belongs to the field of carbon material preparation. Background technique [0002] Since 2004, two scientists from the University of Manchester discovered single-layer graphene and won the 2010 Nobel Prize. This new type of carbon material has been a research hotspot in the fields of materials science and physics. Among the preparation methods of graphene, chemical vapor deposition (CVD) is the most promising method to prepare large-area, high-quality graphene. [0003] At the same time, nitrogen-doped graphene has also been widely studied due to its unique electronic and optical properties. In the field of graphene fluorescence, related researches are prepared and characterized by reducing graphene oxide and then doping with nitrogen. However, there is no report on the preparation of graphene by chemical vapor deposition and related studies on fluorescenc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B32/186C09K11/65
CPCC01B2204/02C01B2204/20C01P2002/80C01P2002/82C09K11/65C01B32/186
Inventor 沈永涛郑楠楠冯奕钰封伟
Owner TIANJIN UNIV