Method for preparing flake-shaped NH4V3O8 microcrystalline with microwave-ultrasonic method

A flaky, microwave technology, applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., can solve problems such as side reactions, low product purity, and difficult reactions, and achieve short reaction cycles, high purity, and improved The effect of 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
  • 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 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 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 microwave-ultrasonic method
  • Method for preparing flake-shaped NH4V3O8 microcrystalline with microwave-ultrasonic method
  • Method for preparing flake-shaped NH4V3O8 microcrystalline with microwave-ultrasonic method

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Effect test

Embodiment 1

[0026] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in an appropriate amount of deionized water at 50°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared NH 4 + The concentration is 0.10mol / L of NH 4VO 3 Solution, denoted as A solution;

[0027] 2) Use 4mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 4.0, obtains B solution;

[0028] 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-ultrasonic synthesis mode is used to make microwave and ultrasonic wave act on the solution simultaneously, wherein the power of microwave is controlled at 200W, and the power of ultrasonic wave is controlled at 600W. Select the temperature-time working mod...

Embodiment 2

[0031] 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 0.20mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0032] 2) Use 3mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 4.5, 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); the microwave-ultrasonic synthesis mode is used to make microwave and ultrasonic wave act on the solution at the same time, wherein the power of microwave is controlled at 300W, and the power of ultrasonic wave is controlled at 400W. Select the temperature-time working mode, turn on the mi...

Embodiment 3

[0039] 1) The analytically pure ammonium metavanadate (NH 4 VO 3 ) was dissolved in deionized water at 55°C, stirred magnetically for 0.5h to dissolve ammonium metavanadate, and prepared into NH 4 + The concentration is 0.12mol / L of NH 4 VO 3 Solution, denoted as A solution;

[0040] 2) Use 3mol L -1 The hydrochloric acid solution adjusts the pH value of A solution to be 5.0, obtains B solution;

[0041] 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-ultrasonic synthesis mode is used to make the microwave and ultrasonic wave act on the solution at the same time, wherein the power of the microwave is controlled at 300W, and the power of the ultrasonic wave is controlled at 300W. Select the temperature-time working mode, tu...

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Abstract

The invention discloses a method for preparing flake-shaped NH4V3O8 microcrystalline with a microwave-ultrasonic method. The method includes the steps that ammonium metavanadate is dissolved in deionized water to prepare an NH4VO3 solution with the NH4+ concentration being 0.05-0.20mol / L, and then the PH value of the solution is adjusted to be 4.0-5.5 to obtain a solution B; by adopting a microwave-ultrasonic synthesis mode, microwaves and ultrasonic waves are made to have effects on the solution B, and the temperature is raised to be 40-80 DEG C to obtain suspension liquid; the suspension liquid is separated in a centrifugal mode to obtain powder products, and then drying and grinding are performed. The NH4V3O8 microcrystalline prepared with the method is uniform in chemical composition, high in purity and uniform in morphology, the thickness of the obtained flake-shaped NH4V3O8 microcrystalline is about 100-200nm, and the electrochemical properties of the material is effectively improved. The preparation method is simple, low in reaction temperature, short in reaction period, high in yield, environmentally friendly and suitable for large-scale production, and no subsequent processing is needed.

Description

technical field [0001] The present invention relates to a preparation method of lithium-ion secondary battery cathode material, in particular to a preparation method of thin-sheet NH by microwave-ultrasound 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 discov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
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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