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Preparation method of high-activity composite electrode material of Co3S4 and graphene

A graphene composite, electrode material technology, applied in battery electrodes, solid electrolyte fuel cells, circuits, etc., can solve the problems of inconvenient control of reaction ratio, large particle size, expensive catalyst, etc., to achieve low cost, enhanced battery performance, The effect of mild process conditions

Active Publication Date: 2015-07-22
SUIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the invention is to provide a kind of highly active Co 3 S 4 The preparation method of the composite electrode material with graphene solves the preparation of Co in the prior art 3 S 4 The catalysts and graphene composite electrode materials are expensive, the particle size is large, the reaction ratio is inconvenient to control and the process is complicated.

Method used

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  • Preparation method of high-activity composite electrode material of Co3S4 and graphene
  • Preparation method of high-activity composite electrode material of Co3S4 and graphene
  • Preparation method of high-activity composite electrode material of Co3S4 and graphene

Examples

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Embodiment 1

[0017] Example 1: A highly active Co 3 S 4 The preparation method of composite electrode material with graphene is specifically completed according to the following steps:

[0018] 1. Preparation of graphene oxide: Take 100 mg of graphite oxide, add 80 mL of ethylene glycol, and sonicate at a frequency of 20 kHz for 1.5 hours. Centrifuge, discard unexfoliated graphite oxide, and obtain a graphene oxide solution;

[0019] 2. Preparation of graphene oxide and cobalt hydroxide turbid solution: add NH dropwise to the graphene oxide solution 3˙ h 2 After adjusting the pH to 8, add cobalt chloride and sonicate for 20 minutes. Control the mass ratio of graphene oxide and cobalt hydroxide added to be 1:10;

[0020] 3. Stir at a constant speed and age: stir for 15-20 hours and age for 12 hours. The temperature is controlled at 30°C;

[0021] 4. Add reducing agent thiourea to the suspension obtained in step 3, and after ultrasonication at 30 kHz for 15 min, control temperature ...

Embodiment 2

[0025] Example 2: A highly active Co 3 S 4 The preparation method of composite electrode material with graphene is specifically completed according to the following steps:

[0026] 1. Preparation of graphene oxide: Take 100 mg of graphite oxide, add 90 mL of ethylene glycol, and sonicate at a frequency of 30 kHz for 1 hour. Centrifuge, discard unexfoliated graphite oxide, and obtain a graphene oxide solution;

[0027] 2. Preparation of graphene oxide and cobalt hydroxide turbid solution: add NH dropwise to the graphene oxide solution 3˙ h 2 After adjusting the pH to 9, add cobalt chloride and sonicate for 15 minutes. Control the mass ratio of graphene oxide and cobalt hydroxide added to be 1:5;

[0028] 3. Stir at a constant speed and age: stir for 15 to 20 hours, and age for 10 hours. The temperature is controlled at 40°C;

[0029] 4. Add reducing agent thiourea to the suspension obtained in step 3, sonicate at a frequency of 20 kHz for 10 minutes, control the temper...

Embodiment 3

[0033] Example 3: A highly active Co 3 S 4 The preparation method of composite electrode material with graphene is specifically completed according to the following steps:

[0034]1. Preparation of graphene oxide: Take 100 mg of graphite oxide, add 100 mL of ethylene glycol, and sonicate at a frequency of 40 kHz for 0.5 hours. Centrifuge, discard the unexfoliated graphite oxide, and obtain a graphene oxide solution;

[0035] 2. Preparation of graphene oxide and cobalt hydroxide turbid solution: add NH dropwise to the graphene oxide solution 3˙ h 2 After adjusting the pH to 10, add cobalt chloride and sonicate for 15 minutes. Control the mass ratio of graphene oxide and cobalt hydroxide added to be 3:10;

[0036] 3. Stir at a constant speed and age: stir for 15 to 20 hours, and age for 10 hours. The temperature is controlled at 50°C;

[0037] 4. Add reducing agent thiourea to the suspension obtained in step 3, and after ultrasonication at 40 kHz for 10 min, control tem...

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Abstract

The invention discloses a preparation method of a high-activity composite electrode material of Co3S4 and graphene. The preparation method comprises the following steps: (1) preparing graphene oxide; (2) preparing an emulsion of graphene oxide and cobalt hydroxide; (3) uniformly stirring the prepared emulsion and performing aging; (4) preparing the composite electrode material of Co3S4 and graphene. The preparation method disclosed by the invention has the advantages that (1) through the adoption of the preparation method, the synthesis of the high-activity composite electrode material of Co3S4 and graphene is realized; (2) the synthesis technology is simple, the technology conditions are moderate, the operation is convenient, and the cost is low; (3) the preparation method disclosed by the invention has universality and offers a new idea for synthesizing other graphene composite materials; (4) the composite electrode material of Co3S4 and graphene, which is prepared by using the preparation method disclosed by the invention, is high in stability, so that the use of poisonous reductant is avoided. The high-activity composite electrode material of Co3S4 and graphene, which is prepared by using the preparation method disclosed by the invention, is suitable for being used as a cathode catalyst for a polymer electrolyte membrane fuel cell (PEMFC), the catalytic activity is significantly improved, and the properties of cells are obviously improved.

Description

technical field [0001] The invention relates to the technical field of composite material preparation, in particular to a highly active Co 3 S 4 Preparation method of composite electrode material with graphene. Background technique [0002] Graphene has the advantages of unique one-dimensional planar structure, large specific surface area, peculiar electronic properties and stability, etc., and is widely used as a catalyst carrier for fuel cells. After compounding graphene with noble metal Pt, it has excellent corrosion resistance and good It has excellent electron conductivity and high electrocatalytic activity, so it is widely used as fuel cell electrode material. Due to the scarcity and high price of precious metal Pt resources, the cost of batteries remains high, which limits the commercialization and large-scale production of PEMFC. Therefore, the study of non-Pt catalysts with low price and high catalytic activity has become an important goal to promote the developm...

Claims

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Application Information

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IPC IPC(8): H01M4/90
CPCH01M4/8647H01M4/88H01M4/9083H01M8/10Y02E60/50
Inventor 赵东江迟彩霞田喜强马松艳董艳萍白晓波田军乔秀丽
Owner SUIHUA UNIV
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