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Multilevel-structured VS4 nano-powder, and preparation method and application thereof

A nano-powder, hydrothermal reaction technology, applied in nanotechnology, structural parts, chemical instruments and methods, etc., can solve the problems of harsh synthesis conditions of vanadium tetrasulfide, difficult to control reaction, slow research progress, etc. High purity and crystallinity, and uniform chemical composition

Active Publication Date: 2016-09-07
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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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  • Multilevel-structured VS4 nano-powder, and preparation method and application thereof
  • Multilevel-structured VS4 nano-powder, and preparation method and application thereof
  • Multilevel-structured VS4 nano-powder, and preparation method and application thereof

Examples

Experimental program
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Effect test

preparation example Construction

[0022] A multilevel structure VS 4 The preparation method of nanopowder, comprises the following steps:

[0023] Step 1: Weigh the vanadium source and sulfur source material, dissolve the vanadium source and sulfur source material in 40-80mL deionized water, control the molar ratio of vanadium and sulfur to 1:1-1:2, magnetically stir or ultrasonically disperse for 10 Solution A was obtained after ~60 min, and the concentration of the vanadium source was 0.06-0.6 mol / L. The vanadium source is one or more of sodium metavanadate, sodium vanadate, ammonium metavanadate, vanadium pentoxide and potassium metavanadate. The sulfur source is one or more of thioacetamide, sodium diethylthiocarbamate and sulfur element.

[0024] Step 2: Transfer solution A to the hydrothermal reaction liner, install an external kettle and place it in a homogeneous reactor, control the filling ratio of the hydrothermal reaction to 40-80%, and synthesize at a temperature of 160-200°C Under reaction 12 ~...

Embodiment 1

[0028] Step 1: Weigh sodium metavanadate and thioacetamide, dissolve them in 60mL of deionized water, control the molar ratio of vanadium and sulfur to 1:1, obtain solution A after magnetic stirring for 60min, and the concentration of vanadium source is 0.06mol / L.

[0029] Step 2: Transfer the solution A to the hydrothermal reaction liner, install an external kettle and place it in a homogeneous reactor, control the filling ratio of the hydrothermal reaction to 60%, and react at a synthesis temperature of 180°C for 24 hours.

[0030] Step 3: After the hydrothermal reaction is completed and cooled naturally, the reaction product is taken out, washed 3 times with water and 3 times with alcohol, collected, and dried at 60°C for 12 hours to obtain the multi-level structure VS 4 Nano powder. Wherein, the washing method is suction filtration washing, and the collection method is suction filtration collection.

[0031] from figure 1 It can be seen that all X-ray powder diffractio...

Embodiment 2

[0034] Step 1: Weigh sodium metavanadate and thioacetamide, dissolve in 40mL deionized water, control the molar ratio of vanadium and sulfur to 1:1.5, obtain solution A after ultrasonic dispersion for 10min, and the concentration of vanadium source is 0.1mol / L.

[0035] Step 2: Transfer the solution A to the hydrothermal reaction liner, install an external kettle and place it in a homogeneous reactor, control the filling ratio of the hydrothermal reaction to 80%, and react for 12 hours at a synthesis temperature of 160°C.

[0036]Step 3: After the hydrothermal reaction is completed and cooled naturally, the reaction product is taken out, washed twice with water and twice with alcohol, collected, and dried at 80°C for 6 hours to obtain the multi-level structure VS 4 Nano powder. Wherein, the washing method is suction filtration washing, and the collection method is suction filtration collection.

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Abstract

The invention provides a multilevel-structured VS4 nano-powder, and a preparation method and an application thereof. According to the invention, a vanadium source solution and a sulfur source solution are mixed under stirring, wherein the molar ratio of vanadium to sulfur is controlled at 1:1-1:2, such that a mixed liquid is obtained; the mixed liquid is subjected to a hydrothermal reaction; when the reaction is finished, cooling, washing, collecting and drying are carried out, such that the multilevel-structured VS4 nano-powder is obtained. The process is simple and is easy to control. The prepared VS4 nano-powder has uniform chemical composition and relatively high purity. The nano-powder shows excellent electrochemical performance when used as a lithium / sodium ion battery electrode material. Also, the method overcomes a defect of high temperature of a traditional calcination method, and does not need large equipment and harsh reaction conditions. The raw materials are cheap and are easy to obtain; cost is low; yield is high; no post treatment is needed; and the method is environment-friendly. The method is suitable for large-scale production.

Description

【Technical field】 [0001] The invention relates to a preparation method of a vanadium tetrasulfide nanometer material, in particular to a multilevel structure VS 4 Nanopowder and its preparation method and application. 【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 J M, 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 capa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00B82Y40/00B01J27/04H01M4/58H01G11/30
CPCH01M4/136H01M4/1397H01M4/5815H01M10/0525H01M10/054H01G11/30C01G31/00B01J27/04C01P2002/72C01P2004/03B01J35/23B01J35/39Y02E60/10
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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