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Method for preparing Co9S8 and nitrogen doped carbon composite array electrode

A composite array, nitrogen-doped carbon technology, applied in the direction of electrodes, chemical instruments and methods, electrolysis process, etc., can solve the problems of lack of inherent active sites, small specific surface area of ​​nanoparticles, poor stability, etc.

Active Publication Date: 2019-06-07
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to pure Co 9 S 8 Due to the small specific surface area of ​​nanoparticles, insufficient electrical conductivity, easy aggregation, poor stability in alkaline media, and lack of intrinsic active sites, it is far from enough to use them to achieve dual-functional catalytic performance.

Method used

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  • Method for preparing Co9S8 and nitrogen doped carbon composite array electrode
  • Method for preparing Co9S8 and nitrogen doped carbon composite array electrode
  • Method for preparing Co9S8 and nitrogen doped carbon composite array electrode

Examples

Experimental program
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Effect test

Embodiment 1

[0020] At room temperature, 0.15 M CoCl 2 ∙ 6H 2 O, urea with a mass fraction of 6.25% was dissolved in 40 mL of deionized water. The carbon paper was soaked in the solution and reacted in a water bath at 90 °C for 2 h, cooled naturally to room temperature, the carbon paper was taken out, rinsed with deionized water three times, and dried for later use. Soak the carbon paper prepared above in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 40 mg of dopamine, stir at room temperature for 24 h, rinse the sample three times with deionized water and dry it. The carbon paper was put into a tube furnace, reacted at 350 °C for 2 h under the airflow of thiourea (0.2 g), then continued to heat up to 700 °C for 2 h, cooled naturally to room temperature and took it out to obtain CFP / Co 9 S 8 @C in situ electrodes.

[0021] figure 1 The OER and ORR linear voltammetry sweep (LSV) diagrams of the electrode prepared in Example 1. It can be seen from the figure t...

Embodiment 2

[0025] At room temperature, 0.15 M CoCl 2 ∙ 6H 2 O, 6.25% urea was dissolved in 40 mL deionized water. The carbon paper was soaked in the solution and reacted in a water bath at 90 °C for 2 h, cooled naturally to room temperature, the carbon paper was taken out, rinsed with deionized water three times, and dried for later use. Soak the carbon paper prepared above in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 30 mg of dopamine, stir at room temperature for 24 h, rinse the sample three times with deionized water, and then dry it. The carbon paper was put into a tube furnace, reacted at 350 °C for 2 h under the airflow of thiourea (0.2 g), then continued to heat up to 700 °C for 2 h, cooled to room temperature naturally, and took out to obtain CFP / Co 9 S 8 @C in situ electrodes.

[0026] Figure 4The OER and ORR linear voltammetry sweep (LSV) diagrams of the electrode prepared in Example 2. It can be seen from the figure that when the current de...

Embodiment 3

[0028] At room temperature, 0.15 M CoCl 2 ∙ 6H 2 O, 6.25% urea was dissolved in 40 mL deionized water. Soak the carbon paper in the solution and react it in a 90°C water bath for 2 hours, cool it down to room temperature naturally, take out the carbon paper, rinse it with deionized water three times, and dry it for later use. Soak the carbon paper prepared above in 50 mL of Tris base with a concentration of 0.01 M and a pH of 8.5, add 50 mg of dopamine, stir at room temperature for 24 h, rinse the sample three times with deionized water, and then dry it. The carbon paper was put into a tube furnace, reacted at 350 °C for 2 h under the air flow of thiourea (0.2 g), then continued to heat up to 700 °C for 2 h, cooled naturally to room temperature and took it out to obtain CFP / Co 9 S 8 @C in situ electrodes.

[0029] Figure 5 The OER and ORR linear voltammetry (LSV) diagrams of the electrode prepared in Example 3. It can be seen from the figure that when the current densi...

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Abstract

The invention provides a method for preparing a bifunctional Co9S8 and nitrogen doped carbon composite array electrode. The method comprises the steps of preparing an alkali type cobalt salt needle-shaped array in-situ electrode by a chemical bath deposition method, then, growing polydopamine on the surface of an alkali type cobalt salt array by using dopamine, then, adding thiourea in a protective atmosphere, and carrying out a vulcanization reaction by a CVD method, wherein during the reaction, the polydopamine is converted into a nitrogen doped carbon material, and an alkali type cobalt salt is converted into Co9S8 in a thiourea atmosphere. The product obtained by the method provided by the invention has a variety of high-electrocatalytic-activity loci, including nitrogen doped active sites in the carbon material and other crystal lattice defects resulting from the nitrogen doped active sites, thereby having excellent electrocatalytic oxygen reduction reaction (ORR) performance; theCo9S8 has a relatively good electrocatalytic oxygen evolution reaction (OER) performance; and furthermore, a heterojunction formed by the Co9S8 and the carbon material also has excellent electrocatalytic OER and OER performance.

Description

technical field [0001] The invention relates to an in-situ electrode and its preparation, and belongs to the field of energy storage and conversion materials and devices. Background technique [0002] With the growing demand for clean and sustainable energy, it is a scientific challenge for modern society to develop low-cost, highly active, and durable renewable energy technologies such as fuel cells and metal-air batteries. It is worth noting that realizing these advanced technologies in our daily life is highly dependent on a series of electrochemical reactions, such as oxygen evolution reaction (OER) and oxygen reduction reaction (ORR). However, these oxygen-based electrochemical reactions are limited by slow kinetics and efficiencies in renewable energy technologies. Noble metal-based electrocatalysts discovered so far (such as Pt / C, RuO 2 , Ir / C) have high catalytic activity for ORR or OER. However, none of the commercial catalysts can perform both reactions satisfac...

Claims

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Application Information

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IPC IPC(8): C25B11/06C25B1/02B01J27/043
Inventor 黄妞闫术芳曹星明
Owner CHINA THREE GORGES UNIV
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