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Silk-derived nitrogen-doped graphene fibers

A graphene fiber and silk fiber technology, applied in electrical components, battery electrodes, circuits, etc., can solve problems affecting the oxygen reduction electrocatalytic activity of materials, performance discounts, and biomass carbon-nitrogen materials stability and followability. , to achieve the effect of favorable diffusion and gas desorption, high specific surface area, high porosity

Inactive Publication Date: 2016-08-10
ZHEJIANG SCI-TECH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

So far, carbon-based oxygen reduction electrocatalytic materials prepared from biomass have been developed to some extent, but there are still many problems. First, the selection of biomass, carbonization methods, and evaluation methods for the electrocatalytic performance of the obtained materials ; Second, the stability and traceability of biomass carbon and nitrogen materials in acidic and alkaline environments; Third, explore the factors such as the number and ratio of doping atoms and the electronic structure of materials that may affect the electrocatalytic activity of materials for oxygen reduction
Most carbon materials are usually only suitable for catalyzing the oxygen reduction reaction in alkaline conditions, and their performance is greatly reduced in acidic media, which seriously affects the large-scale application of fuel cells

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Its preparation method of nitrogen-doped graphene-like fiber derived from silk comprises the steps:

[0030] (1) Pretreatment: Put the silk fiber (mulberry silkworm) in deionized water, soak it for 3 hours and rinse it repeatedly for 3 times, then put it into a vacuum oven for drying, and set the temperature of the oven at 60°C for 6 hours.

[0031] (2) Activation: Soak the dried silk fibers of step (1) in saturated potassium chloride solution for 3 hours, rinse with deionized water 3 times after the end and put them into a vacuum oven for drying. The oven temperature is set at Dry at 60°C for 6 hours.

[0032] (3) Carbonization: put the dried silk fiber in step (2) into a corundum boat, and then place the corundum boat in the middle of the tube furnace. Turn on the protective gas for the silk fibers to make the tube furnace reach a vacuum state and start to heat up; the protective gas is formed by mixing 90% of inert gas (argon) and 10% of reducing gas (ammonia). Rai...

Embodiment 2

[0034] Its preparation method of nitrogen-doped graphene-like fiber derived from silk comprises the steps:

[0035] (1) Pretreatment: Put the silk fiber (tussah) in deionized water, soak it for 6 hours and rinse it repeatedly for 3 times, then put it into a vacuum oven for drying, and set the temperature of the oven at 60°C for 6 hours.

[0036] (2) Activation: Soak the dried silk fibers of step (1) in a saturated zinc chloride solution for 24 hours, rinse with deionized water for 3 times and dry in a vacuum oven after the end, and the oven temperature is set at Dry at 60°C for 6 hours.

[0037](3) Carbonization: put the dried silk fiber in step (2) into a corundum boat, and then place the corundum boat in the middle of the tube furnace. The silk fiber is opened with protective gas to make the tube furnace reach a vacuum state and then start to heat up; the protective gas is formed by mixing 99% of inert gas (nitrogen) and 1% of reducing gas (hydrogen). Raise the temperature...

Embodiment 3

[0039] Its preparation method of nitrogen-doped graphene-like fiber derived from silk comprises the steps:

[0040] (1) Pretreatment: Put the silk fiber (cassava silkworm) in deionized water, soak it for 5 hours and rinse it repeatedly for 3 times, then put it into a vacuum oven for drying, and set the temperature of the oven at 60°C for 6 hours.

[0041] (2) Activation: Soak the dried silk fiber in step (1) in a saturated cobalt nitrate solution for 10 hours, rinse it with deionized water for 3 times and dry it in a vacuum oven. The oven temperature is set at 60 °C for 6 hours.

[0042] (3) Carbonization: put the dried silk fiber in step (2) into a corundum boat, and then place the corundum boat in the middle of the tube furnace. The silk fiber is turned on with a protective gas to make the tube furnace reach a vacuum state and then start to heat up; the protective gas is formed by mixing 95% of an inert gas (argon) and 5% of a reducing gas (ammonia). Raise the temperature ...

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Abstract

The invention discloses silk-derived nitrogen-doped graphene fibers. The silk-derived nitrogen-doped graphene fibers are obtained by the steps of activating the pre-processed silk fibers, then carrying out high-temperature carbonization on the fibers, and cooling. According to the graphene fibers, the oxygen reduction catalysis material is prepared by taking the biomass silk fibers as the carbon source, so that the graphene fibers are large in specific surface area and high in porosity, and diffusion and gas desorption can be facilitated; due to the porous structure characteristic, the graphene fibers are relatively high in catalytic activity, acid resistance, alkali resistance and stability; and meanwhile, the graphene fibers are not required to be loaded to an electrode, instead, the graphene fibers can be directly used as a working electrode for carrying out oxygen reduction catalysis.

Description

technical field [0001] The invention relates to an oxygen reduction catalytic material for a fuel cell, in particular to a nitrogen-doped graphene-like fiber derived from silk. Background technique [0002] The energy crisis and environmental pollution are becoming more and more serious, and the development and utilization of clean and renewable energy is becoming more and more important and urgent. Fuel cell is an energy conversion device that directly converts the chemical energy of fuel into electrical energy by chemical reaction. It is a green energy technology and is of great significance to solve the current energy crisis and environmental pollution problems facing the world. However, the reversibility of the oxygen reduction reaction at the fuel cell cathode is low, the exchange current density is small, and the overpotential is high. Therefore, using the cathode oxygen reduction reaction catalyst to reduce the cathode overpotential and improve the battery performanc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/96
CPCH01M4/96Y02E60/50
Inventor 朱罕杜明亮张明姚菊明
Owner ZHEJIANG SCI-TECH UNIV
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