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Preparation method of NH4V3O8 nanorods

A nanorod, solution technology, applied in nanotechnology, chemical instruments and methods, vanadium compounds, etc., can solve the problems of difficult control of the reaction process, occurrence of side reactions, long reaction time, etc., to improve electrochemical performance, uniform heating, etc. , the effect of short preparation cycle

Inactive Publication Date: 2014-01-01
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Preparation method of NH4V3O8 nanorods
  • Preparation method of NH4V3O8 nanorods
  • Preparation method of NH4V3O8 nanorods

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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 evenly, and prepared NH 4 + The concentration is 0.20mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0025] 2) Use 6mol L ‐1 The hydrochloric acid solution adjusts the pH value of A solution to be 2.0, obtains B solution;

[0026]3) Transfer solution B into a reactor lined with polytetrafluoroethylene, control the filling ratio of the reactor to 50%, then seal the reactor with solution B, place it in a microwave hydrothermal reactor, and select In temperature control mode, the temperature is rapidly raised from room temperature to 120 °C at a heating rate of 40 °C / min, and kept for 30 minutes, then cooled to 70 °C, kept for 30 minutes, and then naturally cooled to room temperature, and the reactor was taken out to obtain a suspension;

[0027] 4) Centrifuge the suspension to obtain a powder pro...

Embodiment 2

[0032] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 70°C, stirred by magnetic force for 0.5h to dissolve ammonium metavanadate evenly, and prepared into NH 4 + The concentration is 0.25mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0033] 2) Use 5mol L ‐1 The hydrochloric acid solution adjusts the pH value of A solution to be 2.5, obtains B solution;

[0034] 3) Transfer solution B into a reactor lined with polytetrafluoroethylene, control the filling ratio of the reactor to 50%, then seal the reactor with solution B, place it in a microwave hydrothermal reactor, and select In temperature control mode, the temperature is rapidly raised from room temperature to 140 °C at a heating rate of 40 °C / min, and kept for 10 minutes, then cooled to 90 °C, kept for 30 minutes, and then naturally cooled to room temperature, and the reaction vessel was taken out to obtain a suspension;

[0035] 4) Centrifuge the suspension to ...

Embodiment 3

[0037] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 65°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 4mol L ‐1 The hydrochloric acid solution adjusts the pH value of A solution to be 2.5, obtains B solution;

[0039] 3) Transfer solution B into a reactor lined with polytetrafluoroethylene, control the filling ratio of the reactor to 50%, then seal the reactor with solution B, place it in a microwave hydrothermal reactor, and select In temperature control mode, the temperature is rapidly raised from room temperature to 130°C at a heating rate of 40°C / min, and kept for 20 minutes, then cooled to 80°C, kept for 20 minutes, and then naturally cooled to room temperature, and the reactor is taken out to obtain a suspension;

[0040] 4) Centrifuge the suspension to obtain a powder...

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Abstract

The invention discloses a preparation method of NH4V3O8 nanorods. The method includes the steps that ammonium metavanadate is dissolved in deionized water to prepare an NH4VO3 solution, the solution is transferred into a reaction still after a pH value is adjusted, the reaction still is placed into a microwave hydrothermal reaction instrument after being sealed, and suspension liquid is obtained after having a reaction in a heated mode; the suspension liquid is separated in a centrifugal mode to obtain powder products, then the powder products are respectively soaked with the deionized water and absolute ethyl alcohol and washed repeatedly, and then the soaked and washed powder products are dried and grinded. NH4V3O8 nanocrystalline prepared with the method is uniform in chemical constitution, high in purity, regular in crystal morphology, small in particulate diameter and even in distribution, the diameter of the obtained nanorods is about 70nm, the ratio of the length of the nanorods to the diameter of the nanorods is about (1:5)-(1:10), electrochemical performance of the materials is effectively improved, and the NH4V3O8 nanorods can be used as lithium battery cathode materials. The preparation method of the NH4V3O8 nanorods is easy to operate, low in reaction temperature and short in preparation period.

Description

technical field [0001] The invention relates to a preparation method of a lithium ion secondary battery cathode material, in particular to an NH 4 V 3 o 8 Preparation method of nanorods. 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 o 8 They a...

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 SHAANXI UNIV OF SCI & TECH