Ultra-small VS4/Super P composite nano-powder as well as preparation method and application thereof

A technology of nanocomposite powder and ph value, applied in the direction of non-aqueous electrolyte battery electrodes, electrical components, battery electrodes, etc., can solve the problems of small specific surface area, high cost, etc., achieve large specific surface area, shorten charge transfer, and yield high effect

Active Publication Date: 2018-06-01
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in these hydrothermal reactions, templating agents including graphene, carbon nanotubes, conductive polymers (polythiophene, polypyrrole, and polyaniline) and perylenetetraacid dianhydride are usually introduced, which has a high cost. , synthetic vs 4 Most of them are one-dimensional structures [Rout CS, Kim B-H, Xu X, Yang J, JeongHY, Odkhuu D, et al. Synthesis and characterization of patronite form of vanadiumsulfide on graphitic layer. JAm Chem Soc.2013; 135:8720-5. ]
In addition, the reported pure phase VS 4 Most of them are micron scale, which leads to its small specific surface area

Method used

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  • Ultra-small VS4/Super P composite nano-powder as well as preparation method and application thereof
  • Ultra-small VS4/Super P composite nano-powder as well as preparation method and application thereof
  • Ultra-small VS4/Super P composite nano-powder as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Step 1: Add 1.0g of sodium metavanadate, 3.6g of thioacetamide and 0.3g of Super P into 60ml of deionized water at the same time, stir magnetically at 800r / min for 65min to obtain a semi-clear solution A;

[0039] Step 2: Then add 1.0mol / L ammonia solution dropwise to solution A under magnetic stirring, control the drip rate of ammonia solution to 0.03ml / min, after adding one drop of ammonia solution, stir until the pH value of the solution is stable , and then drop the next drop of ammonia solution until the pH value of the reaction solution is adjusted to 10 to obtain solution B;

[0040] Step 3: Pour the solution B into the reaction liner at a filling ratio of 60% and seal it, install the liner in the outer kettle and fix it, then place it in a homogeneous reactor, and heat the reaction kettle from room temperature to 8r / min. 180℃ hydrothermal reaction for 24h;

[0041] Step 4: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to ...

Embodiment 2

[0048] Step 1: Add 0.8g of sodium metavanadate, 3.5g of thioacetamide and 0.2g of Super P into 58ml of deionized water at the same time, stir magnetically at 1000r / min for 55min to obtain a semi-clear solution A;

[0049] Step 2: Then add 1.15mol / L ammonia solution dropwise to solution A under magnetic stirring, control the drip rate of ammonia solution to 0.04ml / min, after adding one drop of ammonia solution, stir until the pH value of the solution is stable , and then drop the next drop of ammonia solution until the pH value of the reaction solution is adjusted to 9.9 to obtain solution B;

[0050] Step 3: Pour solution B into the reaction liner at a filling ratio of 55% and seal it, install the liner in the outer kettle and fix it in a homogeneous reactor, and heat the reaction kettle from room temperature to 178℃ hydrothermal reaction for 24.5h;

[0051] Step 4: After the hydrothermal reaction is completed, cool the reaction vessel to room temperature naturally. After fiv...

Embodiment 3

[0053] Step 1: Add 1.1g of sodium metavanadate, 3.7g of thioacetamide and 0.4g of Super P into 63ml of deionized water at the same time, stir magnetically at 900r / min for 60min to obtain a semi-clear solution A;

[0054] Step 2: Then add 1.1mol / L ammonia solution dropwise to solution A under magnetic stirring, control the drip rate of ammonia solution to 0.05ml / min, after adding one drop of ammonia solution, stir until the pH value of the solution is stable , and then drop the next drop of ammonia solution until the pH value of the reaction solution is adjusted to 10.1 to obtain solution B;

[0055] Step 3: Pour the solution B into the reaction liner at a filling ratio of 58% and seal it, place the liner in the outer kettle and fix it in a homogeneous reactor, and heat the reaction kettle from room temperature to 100r / min. 185℃ hydrothermal reaction for 23.5h;

[0056] Step 4: After the hydrothermal reaction is completed, the reaction kettle is naturally cooled to room temper...

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Abstract

The invention relates to a preparation method and an application of ultra-small VS4/Super P composite nano-powder. The preparation method comprises the following steps: adding sodium metavanadate, thioacetamide and Super P to deionized water to obtain a solution A; then dropwise adding ammonia water to the solution A to obtain a solution B with pH of 9.8-10.2; pouring the solution B into a reaction lining, and sealing the reaction lining for hydrothermal reaction; washing a reaction product with water and alcohol alternately to obtain the ultra-small VS4/Super P composite nano-powder. The VS4/Super P composite nano-powder is prepared from VS4 nano-spheres and super P nano-spheres through uniform and interactive distribution. The VS4 nano-spheres are uniform in shape and uniform in size andhave diameter of 50-80 nm. The VS4 nano-spheres are prepared from single crystal VS4 flexible nano-rods with diameter of 20 nm and length of 60-100 nm through winding, and the VS4 flexible nano-rodsgrow along the (110) crystal plane orientation. The VS4/Super P composite nano-powder is applied to lithium/sodium ion batteries and photo/electro-catalytic fields and shows excellent electrochemicaland catalytic properties.

Description

technical field [0001] The present invention relates to a VS 4 / Super P composite powder preparation method, specifically relates to a kind of super small VS 4 / SuperP nanocomposite powder and its preparation method and application. Background technique [0002] vs. 4 The rich V valence states, high sulfur content, one-dimensional chain crystal structure, weak inter-chain connections, and large chain spacing make it have extremely high application prospects in the fields of electrochemistry and catalysis [Xu X, Jeong S, Rout CS, Oh P, KoM, Kim H, et al. Lithium reaction mechanism and high rate capability of VS 4 - graphenenanocomposite as an anode material for lithium batteries. J Mater Chem A. 2014; 2:10847-53.]. At the same time, as far as green sulfur vanadite (VS existing in nature 4 ) rich reserves and its potential low cost, VS 4 It has great commercial value in industrial application. However, pure phase vs 4 The synthesis of VS requires precise control of the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/13
CPCH01M4/13H01M4/364Y02E60/10
Inventor 黄剑锋李文斌何枢薇曹丽云任一杰范海鑫畅珣伟王娜
Owner SHAANXI UNIV OF SCI & TECH
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