Preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability

A lithium-ion battery and negative electrode material technology, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of high requirements for sintering equipment, rapid material capacity decay, poor cycle performance, etc., and achieve uniform and complete coating effect. The effect of high battery safety performance and improved electrochemical performance

Inactive Publication Date: 2016-04-27
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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Problems solved by technology

(2) Alloy materials, mainly including Sn-based and Si-based materials; Sn-based and Si-based materials can be combined with multiple Li + Combined, the alloy material has a high capacity, but this type of material has a volume change of more than 300% during the electrochemical reaction, which causes the material to generate a large lattice stress during the cycle, causing the particle fragmentation of the material and from The current collector falls off, resulting in faster capacity decay and poor cycle performance of the material
(3) Transition metal oxide materials, such as Co 3 o 4 , Fe 3 o 4 etc.; the capacity of transition metal oxides is generally 2 to 3 times that of graphite materials, but the material becomes amorphous during the first discharge process, and the M-O metal bond is destroyed due to the effect of the energy barrier, which makes the material appear greatly Polarization phenomenon, low Coulombic efficiency and gradually increasing lithium intercalation voltage make transition metal oxide anode materials have great obstacles in practic

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  • Preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability
  • Preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability
  • Preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability

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[0033] Example 1

[0034] (1) Weigh 4.68g ammonium metavanadate and 12.24g lithium acetate dihydrate according to the molar ratio V:Li=1:3, add them to 50mL deionized water, and disperse to prepare suspension A;

[0035] (2) Weigh 16.81g of citric acid monohydrate according to the molar ratio V: complexing agent=1:2, add it to 150mL of deionized water and stir to obtain a complexing agent solution B with a concentration of 0.1mol / L;

[0036] (3) Control the stirring, add the complexing agent solution B dropwise to the suspension A, and stir to form a clear and transparent solution C at a temperature of 40°C;

[0037] (4) Weigh 0.026g of lithium fluoride according to the molar ratio V:F=1:0.025, add it to the clear and transparent solution C, stir, and raise the temperature to 90℃ to evaporate the solvent deionized water, and then bake it at 120℃ Dry for 24 hours to obtain blue lithium vanadate precursor;

[0038] (5) Grind and pulverize the blue lithium vanadate precursor in Ar / H 2 Pre...

Example Embodiment

[0044] Example 2

[0045] (1) Weigh 4.68g ammonium metavanadate and 14.28g lithium acetate dihydrate according to the molar ratio V:Li=1:3.5, add them to 50mL deionized water to prepare suspension A

[0046] (2) Weigh 16.81g of citric acid monohydrate according to the molar ratio V: complexing agent=1:2, and add it to 150mL of deionized water to obtain complexing agent solution B;

[0047] (3) Control the stirring temperature at 50°C, add the complexing agent solution B dropwise to the suspension A, and form a clear and transparent solution C after stirring;

[0048] (4) Weigh 0.026g of lithium fluoride according to the molar ratio V:F=1:0.025, add it to the clear and transparent solution C in step (3), stir the temperature to 90°C, evaporate the solvent, and bake at 120°C in the air for 24h Obtain a blue lithium vanadate precursor;

[0049] (5) Grind the blue lithium vanadate precursor under the protection of carbon dioxide and pre-fire at 500°C for 5 hours to obtain the gray lithium ...

Example Embodiment

[0050] Example 3

[0051] According to the element molar ratio V: Li=1:3, weigh 4.68g of ammonium metavanadate and 12.24g of lithium acetate dihydrate and add them to 50mL of deionized water to prepare suspension A

[0052] According to the molar ratio V: complexing agent=1:1.5, weigh 12.61g of citric acid monohydrate and add it to 150mL of deionized water to obtain complexing agent solution B;

[0053] Control the stirring temperature at 40°C, add the complexing agent solution B dropwise to the suspension A, and form a clear and transparent solution C after stirring;

[0054] Weigh 0.052g of lithium fluoride according to the molar ratio V:F=1:0.05, add it to the clear and transparent solution C, stir the temperature to 90℃, evaporate the solvent, and bake it in the air at 100℃ for 24h to obtain blue lithium vanadate Precursor;

[0055] The blue lithium vanadate precursor was ground and pre-fired at 500°C for 5 hours under Ar protection to obtain a gray lithium vanadate precursor;...

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Abstract

The invention provides a preparation method for lithium ion battery cathode material fluorine-doped lithium vanadate with circulatory stability. The preparation method includes adding a vanadium source and a lithium source into deionized water to perform dispersion to obtain suspension A; adding complexing agent into the deionized water to obtain complexing agent liquor B; dripping the complexing agent liquor B into the suspension A to obtain clarified transparent liquor C; adding a fluorine source into the liquor C, and stirring, evaporating and drying the liquor C to obtain a blue lithium vanadate precursor; pre-sintering the blue lithium vanadate precursor in reducing atmosphere or inert atmosphere after grinding and smashing to obtain a grey lithium vanadate precursor; pre-sintering the grey lithium vanadate precursor in reducing atmosphere or inert atmosphere after grinding and smashing to obtain the fluorine-doped lithium vanadate. The preparation method has the advantages that fluorine doping and sintering are performed during complexometry-based lithium vanadate synthesis, and accordingly, electrochemical performance and electric conductivity of the material are improved.

Description

technical field [0001] The invention relates to the technical field of lithium battery preparation, in particular to a preparation method of fluorine-doped lithium vanadate, a lithium-ion battery negative electrode material with stable cycle. Background technique [0002] The development of new energy electric vehicles has drawn extensive attention to the research of power lithium-ion batteries, and continuously improving the safety performance and specific capacity of lithium-ion batteries has become a research hotspot. At present, the negative electrode material of power lithium-ion battery is mainly graphite material, but it only combines one Li per mole of C6. + The improvement of its capacity is limited, and at the same time, its lithium intercalation voltage is low, which is similar to the voltage of dendritic elemental lithium formed by the lithium ion lithium ion reaction, resulting in the formation of micro-short circuits inside the material, making lithium ions a...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/485H01M4/62H01M10/0525
CPCH01M4/366H01M4/485H01M4/625H01M10/0525Y02E60/10
Inventor 马守龙
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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