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Preparation method for prismatic NH4V3O8 nanometer crystal

A nanocrystalline and prismatic technology, which is applied in the field of preparation of lithium-ion secondary battery cathode materials, can solve the problems of side reactions, high reaction temperature, and long reaction time, and achieve short reaction cycle, low reaction temperature, and shape uniformity effect

Active Publication Date: 2014-01-01
盐城市聚龙湖商务集聚区发展有限公司
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  • Abstract
  • Description
  • Claims
  • 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; so looking for a low-temperature, easy-to-control, and rapid synthesis of NH 4 V 3 o 8 The method is of great significance to the research and development of high-performance lithium-ion battery cathode materials and sensor materials

Method used

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  • Preparation method for prismatic NH4V3O8 nanometer crystal
  • Preparation method for prismatic NH4V3O8 nanometer crystal

Examples

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Effect test

Embodiment 1

[0024] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.10mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0025] 2) Use 5mol L -1 Hydrochloric acid solution to adjust the A solution p H value is 3.0, obtains B solution;

[0026]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 synthesis mode of microwave-ultraviolet-ultrasound, microwave, ultraviolet lamp and ultrasonic wave are applied to the solution at the same time. Controlled at 300W. Select the temperature-time working mode, turn on the microwave, ultraviolet lamp and ultrasonic wave at the same time, ...

Embodiment 2

[0031] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 63°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.20mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0032] 2) Use 4mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 3.5, obtains B solution;

[0033] 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 synthesis mode of microwave-ultraviolet-ultrasound, microwave, ultraviolet lamp and ultrasonic wave are applied to solution B at the same time. The power is controlled at 300W. Select the temperature-time working mode, turn on the microwave, ultraviolet lamp and ultrasonic wave ...

Embodiment 3

[0036] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 66°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.25mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0037] 2) Use 4mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 4.0, obtains B solution;

[0038] 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 microwave-ultraviolet-ultrasonic synthesis mode, microwave, ultraviolet lamp and ultrasonic wave are applied to solution B at the same time. The power is controlled at 300W. Select the temperature-time working mode, turn on the microwave, ultraviolet lamp and ultrasonic wave at the ...

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Abstract

Disclosed is a preparation method for a prismatic NH4V3O8 nanometer crystal. Ammonium metavanadate is dissolved in deionized water to obtain an NH4VO3 solution; after the pH value is regulated, the solution is poured into a vessel, the vessel is placed into a microwave-ultraviolet-ultrasonic combined extraction reaction instrument, the temperature rises to be 40-80 DEG C in a microwave-ultraviolet-ultrasonic combined mode and then kept, and suspension liquid is obtained; centrifugal separation is carried out on the suspension liquid to obtain the NH4V3O8 nanometer crystal. According to the preparation method for the prismatic NH4V3O8 nanometer crystal, microwave, ultraviolet and ultrasonic can all provide energy for chemical reaction and promote uniform, rapid and complete conduction of the chemical reaction. The NH4V3O8 nanometer crystal prepared through the method is uniform in shape and granule diameter, and prismatic, the granule diameter is 100-150nm, and the NH4V3O8 nanometer crystal can be used as cathode materials for a lithium ion secondary battery. The preparation method is simple, low in reaction temperature, short in reaction period, simple in process equipment, free of subsequent processing, friendly to the environment and suitable for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion secondary battery cathode material, in particular to a prismatic NH 4 V 3 o 8 Methods of preparing nanocrystals. 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 research of LiV 3...

Claims

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Application Information

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IPC IPC(8): H01M4/58B82Y40/00
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 盐城市聚龙湖商务集聚区发展有限公司
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