Preparation method for carbon-coated lithium vanadate used as negative electrode material of lithium ion battery

A carbon-coated technology for lithium vanadate and lithium ion batteries, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problems of rapid material capacity decay, increased lithium intercalation voltage, poor electronic conductivity, etc., and achieves improved conductivity. rate, grain size reduction, batch stability

Inactive Publication Date: 2016-06-29
HEFEI GUOXUAN HIGH TECH POWER ENERGY
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  • Summary
  • Abstract
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  • Application Information

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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 practical application.
But Li 3 VO 4 It also has its own defects, and its electronic conductivity is very poor, which leads to its poor cycle stability during cycling

Method used

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  • Preparation method for carbon-coated lithium vanadate used as negative electrode material of lithium ion battery
  • Preparation method for carbon-coated lithium vanadate used as negative electrode material of lithium ion battery
  • Preparation method for carbon-coated lithium vanadate used as negative electrode material of lithium ion battery

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Effect test

Embodiment 1

[0032] According to the molar ratio of EDTA: ammonia=1:4, weigh 17.53g of EDTA and add it to 300mL of deionized water, measure 16mL of 25% ammonia water and add it to the EDTA suspension to form a clear and transparent EDTA diamine aqueous solution;

[0033] According to the molar ratio V:Li=1:3, weigh 4.68g ammonium metavanadate and 5.04g lithium hydroxide monohydrate into the EDTA diamine aqueous solution, stir at a temperature of 40℃ to form a yellow-green transparent solution;

[0034] The yellow-green transparent solution was heated to 80°C to evaporate, and after removing the solvent, the blue lithium vanadate precursor was obtained after baking in the air at 120°C for 24 hours;

[0035] Grind the blue lithium vanadate precursor in N 2 / H 2 Pre-fired at 400°C for 4 hours under the protection of mixed gas to obtain a gray lithium vanadate precursor; then grind and crush the gray lithium vanadate precursor and sinter it at 700°C for 8 hours under the protection of high-purity ...

Embodiment 2

[0041] According to the molar ratio of EDTA: ammonia = 1:5, add EDTA to 300 mL of deionized water, and then add ammonia with a mass concentration of 28% to form a clear and transparent EDTA diamine aqueous solution;

[0042] According to the molar ratio V:Li=1:3.5, the V 2 O 5 Add lithium nitrate to the EDTA diamine solution and stir at 30°C to form a yellow-green transparent solution;

[0043] The yellow-green transparent solution is heated to 70°C to evaporate the solvent, and the blue lithium vanadate precursor is obtained after baking in the air at 80°C for 24 hours;

[0044] The blue lithium vanadate precursor was ground and pre-fired at 500°C for 6 hours under the protection of hydrogen to obtain the gray lithium vanadate precursor; the gray lithium vanadate precursor was ground and crushed under the protection of high-purity nitrogen at 900°C After sintering for 6 hours, the carbon-coated lithium vanadate can be obtained after natural cooling.

Embodiment 3

[0046] According to the molar ratio of EDTA: ammonia=1:4.5, weigh 17.53g of EDTA and add it to 300mL of deionized water, measure 18mL of 28% mass fraction of ammonia water and add it to the EDTA suspension to form a clear and transparent EDTA diammonium water solution;

[0047] According to the molar ratio V:Li=1:3, weigh 4.68g of ammonium metavanadate and 12.24g of lithium acetate dihydrate into the EDTA diamine aqueous solution, stir at 50°C to form a yellow-green transparent solution;

[0048] The yellow-green transparent solution is heated to 90°C to evaporate the solvent, and the blue lithium vanadate precursor is obtained after baking in the air at 120°C for 12 hours;

[0049] After grinding the blue lithium vanadate precursor under the protection of high-purity nitrogen, it is calcined at 400℃ for 4h to obtain the gray lithium vanadate precursor; the gray lithium vanadate precursor is ground and crushed in CO 2 Under protection, sintering at 600°C for 12 hours and natural c...

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Abstract

The invention relates to a preparation method for a carbon-coated lithium vanadate used as a negative electrode material of a lithium ion battery. EDTA and ammonium hydroxide are added to deionized water and stirred to form a clarified transparent EDTA diamine water solution; a vanadium source and a lithium source are added and stirred to form a yellow green transparent solution; the transparent solution is evaporated and dried to obtain a blue lithium vanadate precursor; and after the precursor is grinded and smashed, the precursor is pre-calcined under a reducing atmosphere or an inert atmosphere, and then the processed precursor is re-smashed and re-sintered to obtain the carbon-coated lithium vanadate. The carbon-coated lithium vanadate prepared by the invention has the characteristics of uniform particles, stable batches, stable electrochemical performance and the like; and meanwhile, the material has a relatively good discharging platform and a relatively bright application prospect in the power battery industry.

Description

Technical field [0001] The invention relates to the technical field of battery preparation, in particular to a preparation method of carbon-coated lithium vanadate as a negative electrode material of a lithium ion battery. Background technique [0002] The development of new energy electric vehicles has brought extensive attention to the research of power lithium-ion batteries, and continuous improvement of the safety performance and specific capacity of lithium-ion batteries has become a research focus. At present, the anode material of power lithium-ion battery is mainly graphite material, but it only combines one Li per mole of C6 + Limiting the increase of its capacity, at the same time, its lithium insertion voltage is relatively low, which is similar to the voltage of lithium ion lithium evolution reaction to form dendritic elemental lithium, resulting in the formation of micro short circuits inside the material, making lithium ions have a safety hazard that cannot be ignor...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525
CPCH01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 马守龙
Owner HEFEI GUOXUAN HIGH TECH POWER ENERGY
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