Preparation method of porous structure ammonium vanadate material

A porous structure, ammonium vanadate technology, applied in structural parts, vanadium oxide, electrical components, etc., can solve the problems of difficult control of the reaction process, occurrence of side reactions, high reaction temperature, etc., and achieve good electrochemical performance and short reaction time , the effect of low reaction temperature

Active Publication Date: 2014-04-09
盐城大数据资产经营管理有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The synthesis of ammonium vanadate by the above precipitation method needs to prepare gel first, and then reflux the mixed solution with urea at 80°C for one week, which has the disadvantages of difficult control of the reaction process, long reaction cycle, and side reactions. The hydrothermal synthesis of NH 4 V 3 o 8 Surfactants are required, and there are disadvantages of relatively high reaction temperature and long reaction time, so a simple, fast and easy-to-control synthetic 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

Method used

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Embodiment 1

[0026] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, and magnetically stirred for 1 hour to dissolve the ammonium metavanadate evenly to obtain NH 4 + The concentration is 0.10mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0027] 2) Use 5mol L -1 dilute hydrochloric acid to adjust the pH value of the A solution to 1.5, and then carry out the sonochemical reaction of the A solution after adjusting the pH value under the ultrasonic power of 400W for 1 hour to obtain the B solution;

[0028] 3) Pour the B solution into the reactor, let the microwave and the ultraviolet lamp act on the B solution at the same time, wherein the wavelength of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 500W, and the microwave power is controlled at 400-600W, and the platinum resistance is used for temperature measurement , after raising the temperature from room temperature to 90 °C at a heating rate of 15 °C...

Embodiment 2

[0032] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 60°C, and magnetically stirred for 1 hour to dissolve the ammonium metavanadate evenly to obtain NH 4 + The concentration is 0.08mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0033] 2) Use 4mol·L -1 dilute hydrochloric acid to adjust the pH value of the A solution to 2.0, and then perform a sonochemical reaction under 400W ultrasonic power for 0.5h to obtain the B solution;

[0034] 3) Pour the B solution into the reactor, and let the microwave and the ultraviolet lamp act on the solution at the same time, wherein the wavelength of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 500W, and the microwave power is controlled at 400-600W, and the platinum resistance is used for temperature measurement. After raising the temperature from room temperature to 80 °C at a heating rate of 15 °C / min, keep it warm for 30 min, and then naturally cool to r...

Embodiment 3

[0037] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred magnetically for 0.75h to dissolve ammonium metavanadate evenly, and NH 4 + The concentration is 0.06mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0038] 2) Use 3mol L -1 dilute hydrochloric acid to adjust the pH value of the A solution to 2.50, and then perform a sonochemical reaction under 300W ultrasonic power for 0.5h to obtain the B solution;

[0039] 3) Pour the B solution into the reactor, and let the microwave and the ultraviolet lamp act on the solution at the same time, wherein the wavelength of the ultraviolet lamp is 365nm, the power of the ultraviolet lamp is 500W, and the microwave power is controlled at 400-600W, and the platinum resistance is used for temperature measurement. After raising the temperature from room temperature to 70 °C at a heating rate of 15 °C / min, keep it warm for 40 min, and then cool it down to room temperature...

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Abstract

The invention provides a preparation method of a porous structure ammonium vanadate material. The preparation method comprises the following steps: dissolving ammonium metavanadate in deionized water so as to obtain a NH4VO3 solution A; adjusting the pH value of the solution A to 1.5-3.0, and then carrying out phonochemistry reaction so as to obtain a solution B; pouring the solution B into a reactor, enabling microwaves and an ultraviolet lamp to simultaneously act on the solution B, heating to 60-90 DEG C, preserving heat, and then naturally cooling to a room temperature; and carrying out centrifugal separation on suspension liquid in the reactor so as to obtain a powder product, washing and drying, thus obtaining the porous structure ammonium vanadate material. The NH4V3O8 microcrystal prepared by the method is uniform in chemical composition and relatively high in purity, is a special porous structure and has good electrochemistry performance when serving as an anode material for a lithium ion battery; the specific area of the material can be effectively enlarged. The preparation method is simple, low in reaction temperature, short in reaction time, environmentally-friendly and suitable for large-scale production; the follow-up treatment is not needed.

Description

technical field [0001] The invention belongs to the field of preparation of positive electrode materials of lithium ion batteries, and relates to a preparation method of positive electrode materials of lithium ion batteries, in particular to a preparation method of ammonium vanadate material with a porous structure. Background technique [0002] Lithium-ion batteries have the advantages of high voltage, high energy density, long cycle life, good safety, and environmental protection. They have broad application prospects and are considered to be the energy storage materials with the most development potential in the market. [0003] NH 4 V 3 o 8 It is a new type of lithium intercalation material, which has a layered structure and belongs to the monoclinic crystal system, P2 1 / m space group. in NH 4 V 3 o 8 structure, V 3 o 8 - Layers are tightly connected along the c-axis, NH 4 + It is between its layers, stabilizing its structure. NH with larger radius 4 + It...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/48C01G31/02
CPCC01G31/02H01M4/58H01M10/0525Y02E60/10
Inventor 黄剑锋曹杉杉欧阳海波曹丽云费杰李翠艳吴建鹏卢靖
Owner 盐城大数据资产经营管理有限公司
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