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Three-dimensional nitrogen-doped graphene composite material as well as preparation method and application thereof

A technology of nitrogen-doped graphene and composite materials, applied in the field of electrochemical biosensing, can solve the problems of complex structure of electrode materials, large specific surface area of ​​graphene, easy agglomeration of graphene, etc., and achieve fast and large electron transfer rate. Effect of specific surface area and simple structure

Inactive Publication Date: 2015-07-15
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in these electrode materials based on oxidized / reduced graphene oxide modification, graphene often requires a substrate electrode (glassy carbon electrode) to support, the structure of the electrode material is relatively complex, and graphene is prone to agglomeration, so it cannot give full play to the graphene ratio. Large surface area and high electrical conductivity

Method used

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  • Three-dimensional nitrogen-doped graphene composite material as well as preparation method and application thereof
  • Three-dimensional nitrogen-doped graphene composite material as well as preparation method and application thereof
  • Three-dimensional nitrogen-doped graphene composite material as well as preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] (1) With nickel foam as the substrate, in hydrogen (flow rate of 20sccm) and argon (flow rate of 20sccm), the substrate is heated from room temperature to 900°C for 10 minutes in a tube furnace, then annealed at a constant temperature for 1 minute, and then closed Hydrogen gas is fed into carbon source methane (flow rate of 1 sccm) and nitrogen source ammonia gas (flow rate of 1 sccm) to stay for 1 min for growth. The volume ratio of methane and ammonia gas is 1:1, and the temperature is lowered to room temperature for 1 min to obtain substrate-containing Three-dimensional nitrogen-doped graphene;

[0033] (2) Transfer the three-dimensional nitrogen-doped graphene obtained in step (1) to 0.1mol / L FeCl 3 After etching for 48 hours, transfer it to a glass Petri dish filled with ultrapure water and soak for a total of 6 times, the first two times for 5 minutes each, and the last four times for 5 minutes each time to obtain three-dimensional nitrogen-doped graphene;

[003...

Embodiment 2

[0037] (1) With nickel foam as the substrate, in hydrogen (flow rate of 200sccm) and argon (flow rate of 400sccm), in a tube furnace, heat the substrate from room temperature to 1000°C for 30 minutes, then anneal at a constant temperature for 5 minutes, and then close Hydrogen gas, feed carbon source methane (flow rate is 10 sccm) and nitrogen source ammonia gas (flow rate is 14 sccm) and stay for 4 minutes to grow, the volume ratio of methane and ammonia gas is 5:7, cool down to room temperature for 25 minutes, and obtain substrate-containing Three-dimensional nitrogen-doped graphene;

[0038] (2) Transfer the three-dimensional nitrogen-doped graphene obtained in step (1) to 1mol / L FeCl 3 Etched for 13 hours, then transferred to a glass petri dish filled with ultrapure water for immersion, a total of 6 times, 20 minutes each time for the first two times, and 8 minutes each time for the last four times, the three-dimensional nitrogen-doped graphene was obtained;

[0039] (3) ...

Embodiment 3

[0045] (1) With nickel foam as the substrate, in hydrogen (flow rate of 1000sccm) and argon (flow rate of 1000sccm), the substrate is heated from room temperature to 1500°C for 60 minutes in a tube furnace and then annealed at a constant temperature for 5 minutes. Hydrogen gas, carbon source methane (flow rate of 100 sccm) and nitrogen source ammonia gas (flow rate of 200 sccm) were introduced to grow for 25 minutes, the volume ratio of methane and ammonia gas was 1:2, and the temperature was lowered to room temperature for 30 minutes to obtain substrate-containing Three-dimensional nitrogen-doped graphene;

[0046] (2) Transfer the three-dimensional nitrogen-doped graphene obtained in step (1) to the nitric acid of 1:5 (analytical pure nitric acid: ultrapure water) for etching for 6 hours, and then transfer to glass culture filled with ultrapure water Soak in a dish for a total of 6 times, the first two times for 60 minutes each time, and the last four times for 30 minutes ea...

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Abstract

The invention discloses a three-dimensional nitrogen-doped graphene composite material as well as a preparation method and an application thereof to electrochemical biosensors. By means of the characteristics such as high specific surface area, good biocompatibility and high conductivity of the three-dimensional nitrogen-doped graphene, the three-dimensional nitrogen-doped graphene composite material is constructed; the preparation method comprises the following steps: obtaining substrate-containing three-dimensional nitrogen-doped graphene by taking a foam material as a substrate and utilizing a chemical vapor deposition (CVD) method in the presence of inert gas, hydrogen, a carbon source and a nitrogen source, and obtaining the three-dimensional nitrogen-doped graphene composite material by etching and cleaning the three-dimensional nitrogen-doped graphene. By compounding the three-dimensional nitrogen-doped graphene with enzyme / non-enzyme materials, corresponding three-dimensional nitrogen-doped graphene composite materials can be obtained; the three-dimensional nitrogen-doped graphene composite materials are prepared into electrodes and have the characteristics of being high in current corresponding sensitivity, good in stability and wide in application range when being used for detecting a plurality of molecules such as glucose, dopamine, paracetamol and the like.

Description

technical field [0001] The invention belongs to the field of electrochemical biosensing, and relates to a three-dimensional nitrogen-doped graphene composite material and its preparation method and application. Background technique [0002] In modern society, electrochemical biosensors have important application significance in the fields of clinical medicine, bioengineering, environmental monitoring, molecular high-sensitivity detection and even biofuel cells. Detection sensitivity and detection limit are important indicators to measure the performance of electrochemical biosensors. Whether the electrochemical biosensor has good detection sensitivity and detection limit depends on whether the electrochemical electrode has good conductivity, specific surface area and biocompatibility. However, traditional glassy carbon electrodes have disadvantages such as poor conductivity, poor biocompatibility, and low specific surface area, which make electrochemical biosensors have low...

Claims

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Application Information

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IPC IPC(8): G01N27/327H01M8/16
CPCY02E60/50
Inventor 冷炫烨肖遥刘继伦
Owner WUHAN UNIV
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