Preparation method of vanadium tetrasulfide nano-powder and application

A nano-powder technology of vanadium tetrasulfide, which is applied in electrochemical generators, electrical components, battery electrodes, etc., can solve the problems of harsh synthesis conditions of vanadium tetrasulfide, slow research progress, difficult to control the reaction, etc., and achieve excellent electrochemical performance. Uniformity in performance, chemical composition, and low cost

Inactive Publication Date: 2016-07-27
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the harsh synthesis conditions and difficult control of the reaction of vanadium tetrasulfide, the research progress on it has been relatively slow.
There are even rare reports on its use as an electrode material for lithium / sodium-ion batteries

Method used

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  • Preparation method of vanadium tetrasulfide nano-powder and application
  • Preparation method of vanadium tetrasulfide nano-powder and application
  • Preparation method of vanadium tetrasulfide nano-powder and application

Examples

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preparation example Construction

[0023] A preparation method of vanadium tetrasulfide nanopowder, comprising the following steps:

[0024] Step 1: Prepare hydrochloric acid solution and sodium hydroxide solution of certain concentration for adjusting the pH value of the reaction solution. The hydrochloric acid solution can also be sulfuric acid solution, and the sodium hydroxide solution can also be ammonia water or potassium hydroxide solution.

[0025] Step 2: Mix the vanadium source solution and the sulfur source solution, the vanadium-sulfur molar ratio is controlled at 1:2 to 1:10, magnetically stir or ultrasonically disperse until the mixed solution is in a semi-clear state to obtain a suspension A, at this time the vanadium source The concentration is 0.06-0.6 mol / L, the pH of the suspension is adjusted to be acidic or weakly alkaline, the pH value is 1-10, and it is completely dissolved to obtain solution B.

[0026] The vanadium source is one or more of sodium metavanadate, sodium vanadate, ammonium...

Embodiment 1

[0033] Step 1: Prepare a 3mol / L hydrochloric acid solution for adjusting the pH value of the reaction solution.

[0034] Step 2: Weigh sodium metavanadate and thioacetamide and dissolve them in deionized water, then mix the vanadium source solution and the sulfur source solution, the molar ratio of vanadium to sulfur is controlled at 1:4, and then at a speed of 700r / min Stir magnetically for 30 minutes until the solution is in a semi-clear state to obtain a suspension A. At this time, the concentration of the vanadium source is 0.1mol / L, and then add hydrochloric acid solution dropwise to the suspension A until the pH value of the solution reaches 1 to obtain a solution B. The magnetic stirring can be replaced by ultrasonic dispersion.

[0035] Step 3: Transfer the solution B to the hydrothermal reaction liner, add an external kettle, place it in a homogeneous reactor, and react at a synthesis temperature of 180°C for 24 hours.

[0036] Step 4: After the hydrothermal reaction...

Embodiment 2

[0040] Step 1: Prepare 5 mol / L hydrochloric acid solution for adjusting the pH value of the reaction solution.

[0041] Step 2: Weigh sodium metavanadate and thioacetamide and dissolve them in deionized water, then mix the vanadium source solution and the sulfur source solution, the molar ratio of vanadium to sulfur is controlled at 1:2, and then at a speed of 700r / min Stir magnetically for 30 minutes until the solution is in a semi-clear state to obtain a suspension A. At this time, the concentration of the vanadium source is 0.06mol / L, and then add hydrochloric acid solution dropwise to the suspension A until the pH value of the solution reaches 7 to obtain a solution B. The magnetic stirring can be replaced by ultrasonic dispersion.

[0042] Step 3: Transfer the solution B to the hydrothermal reaction liner, add an external kettle, place it in a homogeneous reactor, and react at a synthesis temperature of 180°C for 24 hours.

[0043]Step 4: After the hydrothermal reaction ...

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Abstract

The invention provides a preparation method of vanadium tetrasulfide nano-powder and an application. The method comprises the following steps: firstly, mixing a vanadium source solution with a sulfur source solution, stirring the mixture until semi-clear and then adding an acid or alkali solution to adjust the pH of a reaction liquid; transferring the reaction liquid to a homogeneous reaction instruction for hydrothermal reaction; and finally cooling the reacted product and then washing, collecting and drying the product to obtain the vanadium tetrasulfide nano-powder. According to the method, the technology is is simple and easy to control; and the prepared vanadium tetrasulfide nano-powder is uniform in chemical composition and relatively high in purity, and demonstrates excellent electrochemical properties when used as an electrode material for a lithium / sodium-ion battery. Furthermore, the disadvantage of a high temperature of a traditional calcination method is overcome; large equipment and harsh reaction conditions are not needed; and the method is cheap and available in raw material, low in cost, high in productivity, free of after-treatment and friendly to environment, and can be suitable for large-scale production.

Description

【Technical field】 [0001] The invention relates to a preparation method of an ion secondary battery electrode material, in particular to a preparation method and application of a vanadium tetrasulfide nanometer powder. 【Background technique】 [0002] Lithium-ion batteries are widely used in the portable electronics market due to their advantages of high operating voltage, high capacity, low self-discharge and long cycle life. However, the global lithium resources will not be able to effectively meet the huge demand for power lithium-ion batteries [Tarascon JM, Armand M. Issues and challenges facing rechargeable lithium batteries [J]. Nature, 2001, 414 (6861): 359-367]. Due to its rich resources, low cost, and environmental friendliness, sodium-ion batteries are considered to be an ideal choice to replace lithium-ion batteries as power sources for next-generation electric vehicles and supporting power sources for large-scale energy storage power stations. Therefore, high capac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M10/0525H01M10/054
CPCH01M4/5815H01M10/0525H01M10/054Y02E60/10
Inventor 黄剑锋李文斌王海静李瑞梓费杰曹丽云任一杰罗晓敏闻稼宝井宣人
Owner SHAANXI UNIV OF SCI & TECH
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