Method for preparing flake-shaped NH4V3O8 microcrystalline with water bath method

A water-bath, flake-like technology is applied in the field of preparing flake NH4V3O8 microcrystals by the water-bath method, which can solve the problems of difficult control of the reaction process, occurrence of side reactions, and high reaction temperature, and achieves uniform morphology, short reaction period, The effect of low reaction temperature

Active Publication Date: 2014-01-01
盐城大数据资产经营管理有限公司
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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 process is not easy to control, side reactions occur, and the product purity 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 we are 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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  • Method for preparing flake-shaped NH4V3O8 microcrystalline with water bath method
  • Method for preparing flake-shaped NH4V3O8 microcrystalline with water bath method

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Embodiment 1

[0025] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water, 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 After adjusting the pH value of the A solution to 3.5 with hydrochloric acid solution, the sonochemical reaction was carried out at an ultrasonic power of 800W for 0.5h to obtain the B solution;

[0027] 3) Pour solution B into a beaker of suitable size, seal the mouth of the beaker, put it into a digital display constant temperature water bath, adjust the water level, and react in a water bath at 70°C for 90 minutes;

[0028] 4) After the reaction in the water bath, cool down to room temperature naturally, centrifuge the obtained suspension to obtain a powder product, then soak the powder product in deionized water and absolute ethanol for 10 minutes respectively, and repe...

Embodiment 2

[0032] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration is 0.01mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0033] 2) Use 5mol L ‐1 After adjusting the pH value of solution A to 2.0 with a hydrochloric acid solution, a sonochemical reaction was carried out at an ultrasonic power of 400W for 1 hour to obtain solution B;

[0034] 3) Pour the B solution into a beaker of suitable size, seal the mouth of the beaker, put it into a digital constant temperature water bath, adjust the water level, and react in a water bath at 80°C for 60 minutes;

[0035] 4) After the reaction in the water bath, cool down to room temperature naturally, centrifuge the obtained suspension to obtain a powder product, and then soak the product in deionized water and absolute ethanol for 10 minutes respectively, and repeat first w...

Embodiment 3

[0037] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration is 0.03mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0038] 2) Use 2mol L ‐1 After adjusting the pH value of the A solution to 4.0 with hydrochloric acid solution, the sonochemical reaction was carried out at an ultrasonic power of 600W for 0.5h to obtain the B solution;

[0039] 3) Pour the B solution into a beaker of suitable size, seal the mouth of the beaker, put it into a digital constant temperature water bath, adjust the water level, and react in a water bath at 60°C for 120 minutes;

[0040] 4) After the reaction in the water bath, cool down to room temperature naturally, centrifuge the obtained suspension to obtain a powder product, then soak the powder product in deionized water and absolute ethanol for 10 minutes respectively, and repe...

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Abstract

The invention discloses a method for preparing flake-shaped NH4V3O8 microcrystalline with a water bath method. The method includes the steps that ammonium metavanadate is dissolved in deionized water to prepare an ammonium metavanadate solution marked as a solution A; a phonochemical reaction is performed after the PH value of the solution A is adjusted to obtain a solution B; the solution B is reacted for 30-180min at the temperature of 50-95 DEG C to obtain suspension liquid, the suspension liquid is separated in a centrifugal mode to obtain powder products, then the powder products are soaked in deionized water and absolute ethyl alcohol and washed repeatedly, and then drying and grinding are performed to obtain the flake-shaped NH4V3O8 microcrystalline. The method is short in reaction period and low in reaction temperature and does not need post-processing. The method is simple in equipment, convenient to operate, good in repeatability and suitable for large-scale production. The power obtained with the method is uniform in chemical composition, regular and uniform in crystal morphology and high in microcrystalline purity, all the powder is in the shape of a flake, the thickness of the powder is about 1 micron, and the powder can serve as lithium ion secondary battery cathode material.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion secondary battery positive electrode material, in particular to a method for preparing flake NH by using a water bath method. 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 d...

Claims

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Application Information

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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 盐城大数据资产经营管理有限公司
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