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a fibrous ws 2 Preparation method of nano negative electrode material

A negative electrode material, fiber-shaped technology, applied in the field of preparation of fibrous WS2 nano-negative electrode materials, can solve the problems of difficult control of reactant ratio, easy powder agglomeration, high equipment requirements, etc., achieve light agglomeration, avoid agglomeration, charge and discharge The effect of high capacity

Active Publication Date: 2017-10-27
珠海东杰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At the same time, the in-situ evaporation method and chemical vapor deposition method require high equipment and the ratio of reactants is difficult to control, and the prepared WS 2 It is easy to introduce impurities into nanomaterials, and the powder is easy to agglomerate
In addition, the hydrothermal method and solvothermal method need to prepare nanomaterials under high temperature and high pressure environment, and have high requirements for equipment and poor safety.

Method used

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  • a fibrous ws  <sub>2</sub> Preparation method of nano negative electrode material
  • a fibrous ws  <sub>2</sub> Preparation method of nano negative electrode material
  • a fibrous ws  <sub>2</sub> Preparation method of nano negative electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Step 1: Analytical pure sodium tungstate dihydrate (Na 2 WO 4 2H 2 O) dissolved in deionized water, control W 6+ The concentration is 0.005mol / L, and keep stirring until the sodium tungstate dihydrate dissolves, then add citric acid, and control the ratio of the added citric acid to tungsten to n W : n 柠檬酸 = 3: 2, then placed in a 300W ultrasonic cleaner and ultrasonically oscillated for 50 minutes to obtain solution A;

[0025] Step 2: Add the mixture of analytically pure polyethylene glycol 4000 (PEG 4000) and disodium edetate (EDTA) in solution A PEG4000 :m EDTA =5:1), the total amount of control is wt% (wt% PEG4000 +wt% EDTA ) = 10%, and constantly stirred to fully dissolve polyethylene glycol 4000 and disodium edetate, and then put it into a 300W ultrasonic cleaner for ultrasonic oscillation for 50 minutes, and the obtained solution was recorded as solution B;

[0026] Step 3: After reacting and aging solution B in an electric heating constant temperature w...

Embodiment 2

[0032] Step 1: Analytical pure sodium tungstate dihydrate (Na 2 WO 4 2H 2 O) dissolved in deionized water, control W 6+ The concentration of 0.4mol / L, and keep stirring until sodium tungstate dihydrate dissolves, then add citric acid, control the ratio of the added citric acid to tungsten to n W : n 柠檬酸 = 1:9, then placed in a 700W ultrasonic cleaner for 20 minutes of ultrasonic oscillation to obtain solution A;

[0033] Step 2: Add the mixture of analytically pure polyethylene glycol 4000 (PEG 4000) and disodium edetate (EDTA) in solution A PEG4000 :m EDTA =1:4), the total amount of control is wt% (wt% PEG4000 +wt% EDTA ) = 40%, and constantly stirring to fully dissolve polyethylene glycol 4000 and disodium edetate, then put it into a 700W ultrasonic cleaner and ultrasonically vibrate for 10 minutes, and the obtained solution is recorded as solution B;

[0034] Step 3: React and age solution B in an electric heating constant temperature water bath at 90°C for 1 hour, ...

Embodiment 3

[0038] Step 1: Analytical pure sodium tungstate dihydrate (Na 2 WO 4 2H 2 O) dissolved in deionized water, control W 6+ The concentration is 0.2mol / L, and keep stirring until sodium tungstate dihydrate dissolves, then add citric acid, and control the ratio of the added citric acid to tungsten to n W : n 柠檬酸 = 3:7, then placed in a 500W ultrasonic cleaner and ultrasonically oscillated for 30 minutes to obtain solution A;

[0039] Step 2: Add the mixture of analytically pure polyethylene glycol 4000 (PEG 4000) and disodium edetate (EDTA) in solution A PEG4000 :m EDTA =1:1), the total amount of control is wt% (wt% PEG4000 +wt% EDTA ) = 30%, and constantly stirred to fully dissolve polyethylene glycol 4000 and disodium edetate, then put it into a 500W ultrasonic cleaner and vibrate ultrasonically for 30min, and the obtained solution was recorded as solution B;

[0040] Step 3: After reacting and aging solution B in an electric heating constant temperature water bath at 70°...

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Abstract

The invention provides a preparation method of a fibriform WS2 nanometer anode material. The preparation method of the fibriform WS2 nanometer anode material comprises the steps that sodium tungstate dehydrate and citric acid are dissolved in deionized water, so that a solution A is obtained; polyethylene glycol 4000 and ethylene diamine tetraacetic acid are added to the solution A, so that a solution B is obtained; the solution B is made to react and age at the temperature of 40-100 DEG C, then centrifugation is conducted, sediments obtained through centrifugation are washed, dried and ground, and then a WO3 precursor is obtained; after the WO3 precursor and thioacetamide are independently placed in the same vacuum tube type furnace, a sealed reaction is conducted for 0.5-4 h, after the reaction is ended, a product is cooled naturally to the room temperature, the product is taken out and ground, and then fibriform WS2 nanocrystalline is obtained. The prepared fibriform WS2 nanocrystalline is high in purity, uniformity and crystallinity, and when the fibriform WS2 nanocrystalline is used as the anode material of the sodium-ion battery, the charging capacity and discharging capacity are high.

Description

technical field [0001] The invention relates to a method for preparing fibrous WS 2 The method of nano negative electrode material, especially relates to a kind of template agent assisted water bath-low temperature vacuum reduction crystallization method to prepare fibrous WS 2 A method for an anode material for a sodium-ion battery. Background technique [0002] WS 2 The crystal structure and MoS 2 Similarly, it is also a hexagonal close-packed layered structure. There are strong chemical bonds between tungsten atoms and sulfur atoms, while interlayer sulfur atoms are connected by weak molecular bonds. The binding force between layers is still van der Waals force, and MoS 2 Compared to WS 2 The layer spacing is larger, and the friction coefficient is lower, between 0.03 and 0.05. [0003] WS 2 Insoluble in almost all media, including water, oils, alkalis and almost all acids. But it is sensitive to free gaseous fluorine, hot sulfuric acid and hydrofluoric acid. WS...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/60H01M10/05
CPCH01M4/60H01M10/05Y02E60/10
Inventor 黄剑锋王鑫许占位李嘉胤曹丽云费杰孔新刚欧阳海波姚春燕郝巍
Owner 珠海东杰科技有限公司
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