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Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system

A technology for synthesizing lithium vanadate and mixed solvents, which is applied in chemical instruments and methods, vanadium compounds, inorganic chemistry, etc., to achieve the effects of simplifying synthesis steps, easy control of product particle morphology, and easy control

Active Publication Date: 2016-07-06
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no use of high temperature and high pressure mixed solvothermal system to synthesize lithium vanadate Li 3 VO 4 Related Literature Reports on Single Crystal Micron Powder

Method used

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  • Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system
  • Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system
  • Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 1. Ingredients:

[0037] Mix 60ml of acetone and 40ml of ultrapure water evenly, mix 0.6651g of lithium carbonate and 0.5457g of vanadium pentoxide and disperse them in the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0038]2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0039] Put the sealed reaction kettle into a muffle furnace, heat it to 280°C (the pressure inside the container reaches 9MPa), and keep the temperature constant for 2 hours.

[0040] 3. Cooling:

[0041] The reaction kettle was naturally cooled to room temperature (20° C. to 25° C.), and the reaction kettle was taken out from the muffle furnace.

[0042] 4. Washing:

[0043] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.45 micron in aper...

Embodiment 2

[0048] 1. Ingredients:

[0049] Mix 60ml of acetone and 40ml of ultrapure water evenly, mix 0.6651g of lithium carbonate and 0.5457g of vanadium pentoxide and disperse them in the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0050] 2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0051] Put the sealed reaction vessel into a muffle furnace, heat it to 250°C (the pressure inside the vessel reaches 6.2MPa), and keep the temperature constant for 1 hour.

[0052] 3. Cooling:

[0053] The reaction kettle was naturally cooled to room temperature (20° C. to 25° C.), and the reaction kettle was taken out from the muffle furnace.

[0054] 4. Washing:

[0055] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.45 micron in apert...

Embodiment 3

[0060] 1. Ingredients:

[0061] Mix 50ml of acetone and 50ml of ultrapure water evenly, mix 0.6651g of lithium carbonate and 0.5457g of vanadium pentoxide and disperse them in the above mixed solvent. Then join in the high-temperature and high-pressure reactor (volume is 250 milliliters) that has temperature measurement, pressure measurement device, seal.

[0062] 2. Use high temperature and high pressure mixed solvent thermal system to implement constant temperature reaction:

[0063] Put the sealed reaction kettle into a muffle furnace, heat it to 250°C (the pressure inside the container reaches 6MPa), and keep the temperature constant for 1 hour.

[0064] 3. Cooling:

[0065] The reaction kettle was naturally cooled to room temperature (20° C. to 25° C.), and the reaction kettle was taken out from the muffle furnace.

[0066] 4. Washing:

[0067] The product was taken out from the reaction kettle, and the product was filtered through a vacuum filter (0.22 micron in aper...

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Abstract

The invention discloses a method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with a high-temperature and high-pressure mixed solvent thermal system.The method comprises the steps that solid lithium carbonate powder and solid vanadium pentoxide serve as raw materials, a high-temperature and high-pressure mixed solvent serves as a reaction medium, and the lithium vanadate Li3VO4 monocrystal micrometer powder is synthesized with the condition ranges of 2-9 MPa, 200-350 DEG C and 1-4 h.The method has a unique advantage, the lithium vanadate Li3VO4 monocrystal micrometer powder can be quickly, easily and conveniently obtained, the physical phase is pure, the particle size ranges from 1 micrometer to 20 micrometers, and the dispersibility is good.The synthesizing method is easy, convenient and safe to implement, equipment is convenient to use and simple, the reaction process is easy to control, energy conservation and environment protection are achieved, and the method is especially suitable for industrialized mass production.

Description

technical field [0001] The invention relates to a method for preparing a compound single crystal microstructure that can be used as a lithium ion battery negative electrode material, in particular to a method for synthesizing lithium vanadate Li by using a high temperature and high pressure mixed solvent thermal system. 3 VO 4 Single crystal micropowder method. Background technique [0002] Lithium vanadate Li 3 VO 4 It is a widely used material. Its crystal structure is a non-centrosymmetric structure of pmn21 type, and its nonlinear optical properties have been extensively studied before. Li 3 VO 4 The theoretical capacitance of the battery is 394mAh / g, which has the characteristics of good cycle performance and relatively low charging and discharging potential. It was found that lithium vanadate Li 3 VO 4 It may be a kind of lithium-ion battery negative electrode material with excellent performance. [0003] According to literature reports, lithium vanadate Li ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G31/00
CPCC01G31/00C01P2002/72C01P2004/03C01P2004/10C01P2004/30C01P2004/61
Inventor 李博陶绪堂刘雨桐张梦起
Owner SHANDONG UNIV
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