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Method for preparing cathode material of sodium-ion battery, namely sodium vanadium fluorophosphates

A technology of sodium vanadium fluorophosphate and sodium ion batteries, which is applied to battery electrodes, circuits, electrical components, etc., to achieve good electrochemical performance, low cost, and simple synthesis process

Inactive Publication Date: 2014-02-19
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

When activated carbon is used as the negative electrode, the first charge and discharge specific capacities of the positive electrode material are 82mAh / g and 79mAh / g respectively, the discharge platform is 3.7V, and the capacity decays to 50% of the original after 30 cycles of charge and discharge. NaVPO 4 F material may be used as a practical positive electrode active material for sodium-ion batteries, but its structural stability and comprehensive electrochemical performance still need to be improved through appropriate methods

Method used

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  • Method for preparing cathode material of sodium-ion battery, namely sodium vanadium fluorophosphates

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Embodiment 1

[0024] (1) Mixing materials: use pentavalent vanadium oxy compound, ammonium dihydrogen phosphate, and carbon black as raw materials, dissolve in 80mL deionized water according to the molar ratio of vanadium: phosphorus: reducing agent carbon source element 1:1:1.2, and then Place in a water tank with a constant temperature of 80°C, stir for 6 hours until the solution evaporates to nearly dryness, and obtain a uniformly mixed light green slurry; (2) Pre-calcination: dry the slurry in a vacuum oven, and then transfer it to a tube In the furnace, pre-calcined at 750 ° C for 5 h in a nitrogen atmosphere at a temperature increase rate of 5 ° C per minute, and took it out after cooling to obtain VPO 4 / C precursor; (3) secondary calcination: VPO 4 / C and NaF are mixed according to the stoichiometric ratio, ball milled for 3 hours, sent into a tube furnace, and then roasted at 750°C for 1h in a nitrogen atmosphere at a heating rate of 5°C per minute, and the temperature is lowered w...

Embodiment 2

[0026] Example 2: (1) Mixing: With trivalent vanadium oxy compound, ammonium dihydrogen phosphate, and soluble starch as raw materials, dissolve in 80mL according to the molar ratio of vanadium: phosphorus: reducing agent carbon source element 1:1:1.2 Ionized water, then placed in a water tank with a constant temperature of 80°C, stirred for 6 hours until the solution evaporated to nearly dryness, and a uniformly mixed light green slurry was obtained; (2) pre-calcination: the slurry was dried in a vacuum oven, and then Transfer to a tube furnace, pre-calcined at 650°C for 5h in a nitrogen atmosphere at a rate of 5°C per minute, take it out after cooling, and obtain VPO 4 / C precursor; (3) secondary calcination: VPO 4 / C and NaF were mixed according to the stoichiometric ratio, ball milled for 3 hours, sent into a tube furnace, and then roasted at 650°C for 1h in a nitrogen atmosphere at a heating rate of 5°C per minute, and the temperature was lowered with the furnace to obtai...

Embodiment 3

[0027] Example 3: (1) Mixing materials: use pentavalent vanadium oxy compound, diammonium hydrogen phosphate, and glucose as raw materials, and dissolve in 80mL deionized water, and then placed in a water tank with a constant temperature of 80°C, stirred for 6 hours until the solution evaporated to nearly dryness, and a uniformly mixed light green slurry was obtained; (2) Pre-calcination: dry the slurry in a vacuum oven, and then transfer In a tube furnace, pre-calcined at 850°C for 5 hours in a nitrogen atmosphere at a rate of 5°C per minute, and then taken out after cooling to obtain VPO 4 / C precursor; (3) secondary calcination: VPO 4 / C and NaF are mixed according to the stoichiometric ratio, ball milled for 3 hours, sent into a tube furnace, and then roasted at 850°C for 1h in a nitrogen atmosphere at a heating rate of 5°C per minute, and the temperature is lowered with the furnace to obtain the positive active material NaVPO 4 F / C. Other steps are with embodiment 1.

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Abstract

The invention discloses a method for preparing a cathode material of a sodium-ion battery, namely sodium vanadium fluorophosphates. The method comprises the following steps: using a vanadium source, a phosphorus source and a carbon source as main synthetic raw materials; dissolving into deionized water according to the molar ratio 1:1:1.2 of vanadium: phosphorus: carbon, heating in water bath, and continuously stirring to obtain light green pulp; after vacuum drying, grinding, then transferring into a tube furnace, preburning in an inert atmosphere at a certain temperature rise rate, cooling and then taking out to obtain black VPO4 / C precursor powder; mixing the VPO4 / C with NaF according to a stoichiometric ratio, ball-milling for 3 hours, sending into the tube furnace, then roasting in the inert atmosphere at the certain temperature rise rate, and cooling along with the furnace to obtain a positive active material NaVPO4F / C. According to the invention, cheap and easily-obtained pentavalent vanadium oxide or trivalent vanadium oxide is used as the main raw materials to prepare the sodium vanadium fluorophosphates cathode material through a sol gel activated auxiliary two-step high-temperature solid phase method, and the sodium vanadium fluorophosphates cathode material has the advantages of good stability, uniform particle size and good electrochemical performance. Meanwhile, the method has the advantages of simple synthesis process, short period and low cost and is convenient for large-scale production.

Description

technical field [0001] The invention relates to a preparation method of sodium vanadium fluorophosphate, a positive electrode material of a sodium ion battery, that is, a method for preparing the positive electrode material of a sodium ion battery through a sol-gel-assisted two-stage high-temperature solid-phase method. The method belongs to the technical field of new energy material preparation. Background technique [0002] At present, the research on high-performance lithium-ion batteries and their electrode materials is a hot spot in the fields of electrochemistry, material chemistry, physics, etc., and the properties of sodium ions and lithium ions, which are both the main group I of the periodic table of elements, have many similarities. At this point, it is entirely possible for sodium ions to construct a widely used secondary battery like lithium ions. Moreover, compared with lithium-ion batteries, sodium-ion batteries have lower raw material costs than lithium-ion ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCH01M4/582H01M4/5825Y02E60/10
Inventor 阮艳莉王坤齐平平曹启飞
Owner TIANJIN POLYTECHNIC UNIV
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