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Preparation method for card-shaped NH4V308 micro crystal

A card-shaped, microcrystalline technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve the problems of high reaction temperature, long reaction time, and difficult reaction, and achieve low reaction temperature, simple preparation method, The effect of good electrochemical performance

Active Publication Date: 2014-01-01
盐城抱璞文化传媒有限公司
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Synthesis of NH due to precipitation 4 V 3 o 8 There are disadvantages such as the reaction is not easy to control, side reactions occur, and the purity of the product is low. The hydrothermal method synthesizes NH 4 V 3 o 8 There are disadvantages such as relatively high reaction temperature and long reaction time

Method used

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  • Preparation method for card-shaped NH4V308 micro crystal
  • Preparation method for card-shaped NH4V308 micro crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0025] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 50°C, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration of 0.05mol / L NH 4 VO 3 Solution, denoted as A solution;

[0026] 2) Use 3mol L -1 The dilute hydrochloric acid solution adjusts the pH value of A solution to be 4.5, obtains B solution;

[0027]3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) temperature); the microwave-ultraviolet synthesis mode is adopted, so that the microwave and the ultraviolet lamp act on the solution at the same time, wherein the ultraviolet wavelength of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 300W, and the microwave power is...

Embodiment 2

[0032] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration is 0.10mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0033] 2) Use 4mol L -1 The dilute hydrochloric acid solution adjusts the pH value of A solution to be 4.0, obtains B solution;

[0034] 3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) temperature); the microwave-ultraviolet synthesis mode is adopted to make the microwave and the ultraviolet lamp act on the solution at the same time, wherein the ultraviolet light of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 300W, and the microwave power is c...

Embodiment 3

[0037] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration of 0.15mol / L NH 4 VO 3 Solution, denoted as A solution;

[0038] 2) Use 5mol L -1 The dilute hydrochloric acid solution adjusts the pH value of A solution to be 4.5, obtains B solution;

[0039] 3) Pour solution B into a four-neck round-bottom flask, then put the four-neck round-bottom flask into a microwave-ultraviolet-ultrasonic trinity synthesis extraction reaction apparatus, and fix it, and use direct temperature measurement (platinum resistance measurement) temperature); using the microwave-ultraviolet synthesis mode, the microwave and the ultraviolet lamp act on the solution at the same time, wherein the ultraviolet wavelength of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 300W, and the microwave power is controlled ...

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Abstract

Disclosed is a preparation method for a card-shaped NH4V308 micro crystal. Ammonium metavanadate is dissolved in deionized water to prepare an NH4VO3 solution with the concentration of NH4+ being 0.03-0.15mol / L, and then the pH of the solution is regulated to be 3.5-4.5 to obtain a solution B; microwaves and an ultraviolet lamp simultaneously act on the solution B in a microwave and ultraviolet combined mode, the temperature rises to be at 50-90 DEG C and then is kept, and suspension liquid is obtained; centrifugal separation is carried out on the suspension liquid to obtain powdery products, and then the products are dried. The NH4V308 micro crystal prepared in the method is uniform in chemical composition, is high in purity and is shaped like a card, the thickness of the NH4V308 micro crystal is about 200-500nm, and the NH4V308 micro crystal has good electric chemical performance when serving as anode materials for a lithium ion battery. The preparation method for the card-shaped NH4V308 micro crystal is simple, low in reaction temperature, short in reaction period, without subsequent processing, friendly to the environment, and suitable for large-scale production.

Description

technical field [0001] The present invention relates to a kind of preparation method of anode material of lithium ion secondary battery, especially to a kind of card shape NH 4 V 3 o 8 microcrystalline method. Background technique [0002] Lithium-ion secondary batteries have the advantages of high voltage, high specific energy, long cycle life, stable discharge performance, good safety, no pollution, and wide operating temperature range. They have broad application prospects and become a research hotspot in recent years. [0003] Vanadium is a multivalent metal element among transition elements. It can form a variety of oxides with oxygen, and can also form composite oxides with other cations and oxygen. They generally have the ability to intercalate lithium and can be used as lithium-ion batteries. cathode material, such as V 2 o 5 , LiV 3 o 8 Wait. NH 4 V 3 o 8 is in LiV 3 o 8 A new type of lithium intercalation material discovered on the basis of the researc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/12B82Y40/00C01G31/00H01M4/5825Y02E60/10
Inventor 黄剑锋曹杉杉曹丽云费杰欧阳海波李翠艳吴建鹏卢静
Owner 盐城抱璞文化传媒有限公司
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