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Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof

A technology of carbon-coated lithium iron phosphate and metal titanium, applied in electrical components, battery electrodes, circuits, etc., can solve the problems of low tap density, poor electrical conductivity, material capacity attenuation, etc., and achieve the effect of low cost and high capacity

Inactive Publication Date: 2011-04-13
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] So far, there have been many reports on the synthesis methods of materials. The most researched and most likely to realize industrialization is the high-temperature solid-phase method, but lithium iron phosphate has its inherent shortcomings, such as low lithium ion diffusion coefficient and poor conductivity. etc. Therefore, the materials prepared by the conventional method have disadvantages such as poor electrochemical performance, uneven particle size distribution, and low tap density.
In order to improve the performance of the material, it is generally doped or coated, such as C coating (CN101172599, CN101442117, CN101764205A, CN101777636A), transition metal doping (CN1785799), rare earth doping (CN1830764, CN101630738), etc., The above methods can improve the performance of lithium iron phosphate to a certain extent, but the performance improvement is not too significant

Method used

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  • Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof
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  • Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0023] (1) Accurately weigh 0.025molLi 2 CO 3 , 0.0225molFe 2 o 3 , 0.005molTiO 2 and 0.05molNH 4 h 2 PO 4 Put into the ball mill tank for batching;

[0024] (2) Add the prepared powder into acetone which is 4 times the volume of the powder, and then place it in a ball mill and rotate it at a rate of 250rpm / min for 5h;

[0025] (3) Dry the ground slurry in an oven at 110° C., and then add a saturated aqueous solution containing 2.2 g of citric acid to make a rheological phase precursor;

[0026] (4) Heat the above precursor at a heating rate of 1°C / min under an inert atmosphere, keep the temperature at 100°C for 2 hours, then raise the temperature to 400°C for 5 hours, take it out and grind it after cooling down in the furnace, and press it under a pressure of 200MPa into a compact cylinder;

[0027] (5) Heat up the pressed cylinder to 850°C for 12 hours at a constant temperature in a high-purity nitrogen atmosphere, and then cool down to room temperature with the fur...

Embodiment 2

[0031] (1) Accurately weigh 0.025molLi 2 CO 3 , 0.025molFe 2 o 3 and 0.05molNH 4 h 2 PO 4 Put into the ball mill tank for batching;

[0032] (2) Add the prepared powder into acetone which is 4 times the volume of the powder, and then place it in a ball mill and rotate it at a rate of 250rpm / min for 5h;

[0033] (3) Dry the ground slurry in an oven at 110° C., and then add a saturated aqueous solution containing 2.2 g of citric acid to make a rheological phase precursor;

[0034] (4) Heat the above precursor at a heating rate of 1°C / min under an inert atmosphere, keep the temperature at 100°C for 2 hours, then raise the temperature to 400°C for 5 hours, take it out and grind it after cooling down in the furnace, and press it under a pressure of 200MPa into a compact cylinder;

[0035] (5) The pressed cylinder was heated to 850° C. for 12 h at a constant temperature in an inert atmosphere, and the temperature was lowered to room temperature with the furnace to obtain 8.7 g...

Embodiment 3

[0038] (1) Accurately weigh 0.025molLi 2 CO 3 , 0.02325molFe 2 o 3 , 0.0035molTiO 2 and 0.05molNH 4 h 2 PO 4 Put into the ball mill tank for batching;

[0039] (2) Add the prepared powder into acetone which is 4 times the volume of the powder, and then place it in a ball mill and rotate it at a rate of 250rpm / min for 5h;

[0040] (3) Dry the ground slurry in an oven at 110° C., and then add a saturated aqueous solution containing 2.2 g of citric acid to make a rheological phase precursor;

[0041] (4) Heat the above precursor at a heating rate of 1°C / min under an inert atmosphere, keep the temperature at 100°C for 2 hours, then raise the temperature to 400°C for 5 hours, take it out and grind it after cooling down in the furnace, and press it under a pressure of 200MPa into a compact cylinder;

[0042] (5) The pressed cylinder was heated to 850° C. for 12 h at a constant temperature in an inert atmosphere, and the temperature was lowered to room temperature with the f...

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Abstract

The invention discloses metallic titanium doped carbon-coating lithium iron phosphate and a preparation method thereof, which belong to the technical field of battery material preparation. The lithium iron phosphate has the chemical formula: LiFe1-xTixPO4 / C, wherein x is greater than 0 and is smaller than or equal to 0.2, and the C has the mass percent of 10%. The preparation method comprises thefollow steps of: weighing and proportioning lithium sources, Fe2O3, TiO2 and NH4H2PO4 at the mol ratio of lithium to iron to titanium to phosphorus being 1 to 1-x to x to 1, wherein x is greater than0 and is smaller than or equal to 0.2; then, grinding the materials after acetone addition, adding a saturated aqueous solution of citric acid after drying to be prepared into rheological phase precursor, grinding the precursor for 3 to 6h at the constant temperature of 400 DEG C under inert atmosphere and pressing the ground precursor into tight cylinder bodies; and finally, raising the temperature to 500 to 900 DEG C and roasting for 5 to 15h at the constant temperature to obtain the product. The prepared material has the characteristics of high capacity and high tap density; and the preparation method is simple, has lower cost and is applied to industrial production.

Description

technical field [0001] The invention relates to the technical field of battery material preparation, in particular to metal titanium-doped carbon-coated lithium iron phosphate and a preparation method thereof. Background technique [0002] Lithium-ion battery, as a high-performance green power source, has been widely used in various portable electronic products and communication tools in recent years, and has been gradually developed as a power source for electric vehicles, thus promoting it to a safe, environmentally friendly, low-cost Development in the direction of cost and high specific energy. [0003] Cathode material is a key part that determines the performance of lithium-ion batteries. Today, with more emphasis on safety and environmental protection, lithium iron phosphate has become a research hotspot in various countries. Lithium iron phosphate material is non-toxic, environmentally friendly, rich in raw materials, low in price, good in high temperature stabilit...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M4/1397
CPCY02E60/122Y02E60/12Y02E60/10
Inventor 韩恩山朱令之靳素芳张俊平刘吉云
Owner HEBEI UNIV OF TECH
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