Preparation method of nitrogen-doped graphene/copper sulfide/hollow sulfur composite material

A technology of nitrogen-doped graphene and composite materials, which is applied in the field of nanomaterial synthesis, can solve problems such as slow migration speed, reduced utilization rate of sulfur active materials, and slow electrochemical reaction kinetics, so as to improve electronic conductivity and Ionic conductivity, improving electrochemical performance, and reducing the effect of shuttling effect

Active Publication Date: 2017-07-21
常熟东南高新技术创业服务有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This phenomenon, known as the shuttle effect, reduces the availability of sulfur active species
At the same time insoluble Li 2 S and Li 2 S 2 Deposited on the surface of the lithium negative electrode, which further deteriorates the performance of the lithium-sulfur battery; (3) the final product of the reaction, Li 2 S is also an electronic insulator and will be deposited on the sulfur electrode, while lithium ions migrate slowly in solid lithium sulfide, slowing down the electrochemical reaction kinetics; (4) sulfur and the final product Li 2 The density of S is different. When sulfur is lithiated, the volume expands by about 79%, which easily leads to Li 2 Pulverization of S, causing safety problems in lithium-sulfur batteries
The above deficiencies restrict the development of lithium-sulfur batteries, which is also a key issue that needs to be solved in current research on lithium-sulfur batteries.

Method used

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  • Preparation method of nitrogen-doped graphene/copper sulfide/hollow sulfur composite material
  • Preparation method of nitrogen-doped graphene/copper sulfide/hollow sulfur composite material

Examples

Experimental program
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Embodiment 1

[0020] (1) Add 100g of sulfur powder into carbon disulfide, stir and dissolve to form a solution of 1g / mL;

[0021] (2) 5g of high-purity nickel powder was passed through a high-energy ball mill, ball-milled for 0.5 hours, added to the above solution after ball-milling, stirred to form a uniform suspension, mechanically stirred for 0.5 hours, and spray-dried to form sulfur-coated spherical particles;

[0022] (3) Add spherical particles into 1 mol / L ferric chloride solution, stir and react for 5 hours, wash with water and filter.

[0023] (4) The filtered precipitate was added to a solution containing 10g of copper chloride, 10g of thioacetamide and 1g of sodium dodecylbenzenesulfonate, stirred into a homogeneous suspension, heated to 60°C and stirred for 30 minutes , centrifugation and washing to obtain copper sulfide-coated sulfur particles;

[0024] (5) Add 10 g of nitrogen-doped graphene to water and ultrasonically disperse to form a suspension with a uniform concentratio...

Embodiment 2

[0026] (1) Add 100g of sulfur powder into carbon disulfide, stir and dissolve to form a solution of 5g / mL;

[0027] (2) 20g of high-purity nickel powder was passed through a high-energy ball mill, ball-milled for 2 hours, added to the above solution after ball-milling, stirred to form a uniform suspension, mechanically stirred for 1 hour, and spray-dried to form sulfur-coated spherical particles;

[0028] (3) The spherical particles were added to the 2mol / L ferric chloride solution, stirred and reacted for 1 hour, washed with water and filtered.

[0029] (4) The filtered precipitate was added to a solution containing 20 g of copper chloride, 15 g of thioacetamide and 2 g of sodium dioctyl succinate sulfonate, stirred into a homogeneous suspension, heated to 90°C and stirred for 5 minutes , centrifugation and washing to obtain copper sulfide-coated sulfur particles;

[0030] (5) Add 20 g of nitrogen-doped graphene into water and ultrasonically disperse to form a suspension wit...

Embodiment 3

[0032] (1) Add 100g of sulfur powder to carbon disulfide, stir and dissolve to form a solution of 2g / mL;

[0033] (2) 10g of high-purity nickel powder was passed through a high-energy ball mill, ball-milled for 1 hour, added to the above solution after ball-milling, stirred to form a uniform suspension, mechanically stirred for 0.6 hours, and spray-dried to form sulfur-coated spherical particles;

[0034] (3) The spherical particles were added to the 1.5mol / L ferric chloride solution, stirred and reacted for 3 hours, washed with water and filtered.

[0035] (4) The filtered precipitate was added to a solution containing 15g of copper chloride, 12g of thioacetamide and 1.5g of sodium octadecyl sulfate, stirred into a homogeneous suspension, heated to 70°C and stirred for 15 minutes. Centrifuge and wash to obtain copper sulfide-coated sulfur particles;

[0036] (5) 15g nitrogen-doped graphene was added into water and ultrasonically dispersed to form a suspension with a uniform ...

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Abstract

The invention discloses a preparation method of a nitrogen-doped graphene/copper sulfide/hollow sulfur composite material. The preparation method comprises the following steps: step (1), adding powdered sulfur into carbon dioxide, stirring and dissolving to form a uniform solution; step (2), ball-milling high-purity nickel powder through a high-energy ball grinding mill, adding the high-purity nickel powder after ball-milling into the solution, stirring to form uniform suspension liquid, mechanically stirring, and carrying out spray drying to form sulfur clad spherical particles; step (3), adding the spherical particles into a ferric chloride solution, stirring for reaction, washing and filtering; and step (4), adding a filtered precipitate into a solution containing copper chloride, thioacetamide and a surface active agent, stirring to form uniform suspension liquid, heating and stirring for reaction, centrifuging and washing to obtain copper sulfide clad sulfur particles. In the composite material, a space is reserved for the volume expansion, in the charging and discharging process, of sulfur material through the design of a hollow structure, so that the electrochemical performance can be effectively improved.

Description

technical field [0001] The invention relates to the synthesis of nanomaterials, in particular to a preparation method of a positive electrode material of a lithium-sulfur battery. Background technique [0002] Lithium-sulfur battery is a battery system with metal lithium as the negative electrode and elemental sulfur as the positive electrode. Lithium-sulfur batteries have two discharge plateaus (about 2.4 V and 2.1 V), but their electrochemical reaction mechanisms are complex. Lithium-sulfur batteries have the advantages of high specific energy (2600 Wh / kg), high specific capacity (1675 mAh / g), and low cost, and are considered to be a promising new generation of batteries. However, at present, there are problems such as low utilization rate of active materials, low cycle life and poor safety, which seriously restrict the development of lithium-sulfur batteries. The main reasons for the above problems are as follows: (1) Elemental sulfur is an insulator of electrons and io...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/38H01M4/62H01M10/052B82Y30/00
CPCB82Y30/00H01M4/366H01M4/38H01M4/625H01M4/628H01M10/052Y02E60/10
Inventor 钟玲珑
Owner 常熟东南高新技术创业服务有限公司
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