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Nanometer multilayer mesoporous metal nitride/graphene composite materials for super capacitor and preparation method thereof

A technology of supercapacitors and composite materials, applied in capacitors, electrolytic capacitors, circuits, etc., can solve problems such as poor conductivity and easy aggregation of nanomaterials

Active Publication Date: 2015-06-24
泰州市海通资产管理有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, metal nitrides have two very fatal shortcomings as supercapacitor materials. One is poor conductivity; the other is that nanomaterials are easy to aggregate, which has a huge impact on its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment ( 1

[0018] Add 25g of concentrated sulfuric acid, 2.4g of potassium persulfate, and 2.5g of phosphorus pentoxide into a 500mL container in sequence, stir, slowly raise the temperature to 80°C in a water bath, add 5.0g of graphite, stir for 10 hours, and naturally cool to room temperature. After suction filtration and drying, pre-oxidized graphite was obtained. Add 2.5g of pre-oxidized graphite, 1.3g of sodium nitrite, and 105g of concentrated sulfuric acid into the flask, stir in an ice bath, slowly add 7.5g of potassium permanganate, control the temperature at 0-5°C for 1 hour, and then use 35 ℃ water bath heating, heat preservation reaction for 8 hours, remove the water bath and drop distilled water (T<98 ℃) with a dropper, heat the water bath to 96 ℃, heat preservation reaction for 30 minutes, when the temperature drops to 50-60 ℃, add 7.4 g 5% hydrochloric acid and 5mL 30% hydrogen peroxide, washed with distilled water until neutral, ultrasonic stripping, dialysis, and drying ...

Embodiment ( 2

[0024] The preparation of graphene oxide is with embodiment (1).

[0025] Weigh 50mg of graphene oxide into 40mL of water, then add CTAC 5g, NaOH 0.2g, ultrasonically disperse for 30min, heat up to 40°C, then slowly add 3g of tetraethyl orthosilicate dropwise, react for 8h, centrifuge, wash with ethanol, and dry. Get GO-SiO 2 composite material.

[0026] Weigh 5g GO-SiO 2 In the reaction flask, add 15g ethylenediamine and 50mL carbon tetrachloride, reflux at 90°C for 24h, dry the dark brown solution for 12h, grind it into a fine powder, roast it at 800°C for 6h in a nitrogen atmosphere, and use 5% hydrogen for the product Fluoric acid was dissolved, filtered, washed with ethanol, and dried at 100°C to obtain G-C 3 N 4 composite material.

[0027] Weigh 1.0g G-C 3 N 4 In the reaction bottle, add 15mL ethanol to disperse, then add 5g triethoxymolybdenum, stir, expose to the air for 48h, form a gel, dry, and then bake in a nitrogen atmosphere at 750°C for 6h to obtain G-Mo...

Embodiment ( 3

[0030] The preparation of graphene oxide is with embodiment (1).

[0031] Weigh 20mg of graphene oxide into 20mL of water, then add CTAB 0.5g, NaOH 0.02g, ultrasonically disperse for 30min, heat up to 40°C, then slowly add tetraethyl orthosilicate 0.75g, react for 8h, centrifuge, wash with ethanol, dried to obtain GO-SiO 2 composite material.

[0032] Weigh 0.5g GO-SiO 2 In the reaction flask, add 2.5g ethylenediamine and 7.5mL carbon tetrachloride, reflux at 90°C for 24h, dry the dark brown solution for 12h, grind it into a fine powder, and roast it at 600°C for 5h in an argon atmosphere. % hydrofluoric acid was dissolved, filtered, washed with ethanol, and dried at 100°C to obtain G-C 3 N 4 composite material.

[0033] Weigh 1.0g G-C 3 N 4 In the reaction bottle, add 15mL ethanol to disperse, then add 2.2g triethoxyvanadium, stir, expose to air for 72h, form a gel, dry, and then bake in an argon atmosphere at 650°C for 6h to obtain a G-VN composite Material.

[0034...

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Abstract

The invention relates to multilayer metal nitride / graphene electrochemical super capacitor composite electrode materials and a preparation method thereof. The preparation method of the multilayer metal nitride / graphene electrochemical super capacitor composite electrode materials comprises (1) preparing graphene oxide; (2) self-assembling silicon source on the surface of the oxidized graphene to obtain layered graphene oxide-mesoporous silica composite materials GO-SiO2 under an alkaline condition with a cationic surface active agent as a template agent; (3) roasting carbon tetrachloride and ethylenediamine in inert gas after polymerization with the GO-SiO2 as a template and then removing the SiO2 in the template agent to obtain layered graphene-mesoporous carbon nitride composite materials G-C3N4 and (4) cross-linking a metal precursor on the template agent G-C3N4 and then roasting in inert atmosphere to obtain the multilayer metal nitride / graphene electrochemical super capacitor composite electrode materials. The electrode materials prepared from the method have the advantages of being up to 876 farads per gram in specific capacitance, being capable of remaining over 95% in specific capacitance after charge-discharge cycles for 2000 times, being long in service life and being good in cycling stability.

Description

technical field [0001] The invention relates to a nanometer multilayer metal nitride / graphene composite material for supercapacitor electrode materials and a preparation method thereof, belonging to the technical field of electrochemistry and material synthesis. Background technique [0002] Energy and environmental issues are two major problems that human beings need to solve urgently. Today, with the depletion of fossil energy, increasingly serious environmental pollution, and global warming, it is particularly urgent to seek renewable green energy to replace traditional fossil energy and to seek harmony between man and the environment. The utilization of new renewable energy, such as wind energy and solar energy; the gradual marketization of electric vehicles and hybrid electric vehicles, and the rapid development of various portable electrical devices require efficient, practical, and "green" energy storage and transportation systems . For the new "green" energy storag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01G9/042
CPCY02E60/13
Inventor 秦勇储富强陶永新孔泳黎珊
Owner 泰州市海通资产管理有限公司
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