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Nitrogen and sulfur co-doped three-dimensional graphene and transition metal sulfide composite material, as well as universal preparation method and application thereof

A technology of nitrogen-sulfur co-doping and transition metals, applied in electrochemical generators, electrical components, battery electrodes, etc., to achieve the effects of controllable particles, solving capacity fading, and uniform size

Inactive Publication Date: 2019-06-28
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it remains a great challenge to invent a facile and gentle method for the simultaneous construction of doped 3D carbon materials recombined with transition metal sulfides.

Method used

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  • Nitrogen and sulfur co-doped three-dimensional graphene and transition metal sulfide composite material, as well as universal preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Disperse 0.1g of graphene oxide in a mixed solution of 10ml of deionized water and 10ml of ethanol, then add 0.06g of melamine, 0.085g of thiocyanuric acid and 0.3g of ferric nitrate nonahydrate in sequence, at 50°C Stirring was continued for 30 min. The solution was then transferred to a polytetrafluoroethylene lining for hydrothermal reaction at 120°C / 8h. The sample after the hydrothermal reaction was filtered and washed several times, freeze-dried, and then heated to 650°C at a heating rate of 2°C / min in an argon-protected tube furnace for 1 hour. The flow rate of argon gas during heat treatment is 0 sccm.

Embodiment 2

[0026] Disperse 0.1g of graphene oxide in a mixed solution of 20ml of deionized water and 10ml of ethanol, then add 0.12g of melamine, 0.68g of thiocyanuric acid and 0.5g of cobalt nitrate hexahydrate in sequence, at 70°C Stirring was continued for 100 min. Then transfer the solution to a polytetrafluoroethylene liner for hydrothermal reaction at 150°C / 4h. The sample after the hydrothermal reaction was filtered and washed several times, freeze-dried, and then heated to 750°C at a heating rate of 5°C / min in an argon-protected tube furnace for 1 hour. The flow rate of argon gas during heat treatment is 50 sccm.

Embodiment 3

[0028] Disperse 0.1g of graphene oxide in a mixed solution of 30ml of deionized water and 10ml of ethanol, then add 0.06g of melamine, 0.17g of thiocyanuric acid and 0.8g of nickel nitrate hexahydrate in sequence, at 120°C Stirring was continued for 30 min. The solution was then transferred to a polytetrafluoroethylene lining for hydrothermal reaction at 180°C / 8h. The sample after the hydrothermal reaction was filtered and washed several times, freeze-dried, and then heated to 850°C at a heating rate of 20°C / min in an argon-protected tube furnace for 3 hours. The flow rate of argon gas during heat treatment is 100 sccm.

[0029] refer to figure 1 , figure 1 SEM photographs of samples prepared for this example. The S-4800 scanning electron microscope (SEM) of Japan Electronics Co., Ltd. was used to observe the morphology, and it can be clearly seen that the graphene completely covers the nickel sulfide nanoparticles.

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Abstract

The invention discloses a nitrogen and sulfur co-doped three-dimensional graphene and transition metal sulfide composite material, as well as a universal preparation method and application thereof. According to the invention, the thiocyanuric acid is adopted as a nitrogen and sulfur doping agent, a three-dimensional graphene soft mold agent and a transition metal vulcanizing agent. The hydrothermal-heat treatment method is adopted to realize the simultaneous and in-situ construction of a composite structure of a transition metal sulfide completely coated with doped graphene. The metal sulfideis completely coated with nitrogen and sulfur co-doped graphene. According to the structural design, the problem of capacity attenuation caused by volume expansion of transition metal sulfide in the lithium storage or sodium storage process can be obviously solved. The preparation method is safe in process and easy to operate, wherein the mass production can be achieved. The prepared composite material can be used as a lithium ion battery and sodium ion battery negative electrode active material.

Description

technical field [0001] The invention belongs to the field of electrode materials for lithium-ion batteries and sodium-ion batteries, and relates to a composite material of carbon material coated metal sulfide, in particular to a nitrogen-sulfur co-doped three-dimensional graphene and transition metal sulfide composite material and its general purpose Appropriate preparation methods and applications. Background technique [0002] Transition metal sulfides (MSs) are considered as one of the most promising candidates as anode materials for sodium-ion batteries (SIBs) due to their high theoretical capacity, low cost, and good electronic conductivity. However, the pulverization effect of MSs caused by the volume expansion during the repeated intercalation and desodiation process and the dissolution of reaction intermediate sulfides in the electrolyte will lead to a sharp decrease in the cycle capacity of MSs. Therefore, the research on improving the cycle stability of MSs in Li-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525H01M10/054
CPCY02E60/10
Inventor 黄剑锋席乔李嘉胤曹丽云齐慧王羽偲嘉王璐王芳敏
Owner SHAANXI UNIV OF SCI & TECH
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