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Spherical LiFePO4/(C+La2/3-xLi3xTiO3) composite anode material and preparation method thereof

A positive electrode material and composite technology, applied in the field of spherical LiFePO4/composite positive electrode material and its preparation, can solve the problems of large battery size, inconvenient portability, unreachable lithium ion diffusion rate, unfavorable high rate performance of materials, etc., to achieve Improve electrochemical performance, improve discharge and cycle stability, and prevent corrosion

Inactive Publication Date: 2013-11-20
XIANGTAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, it has obvious defects: on the one hand, due to LiFePO 4 The characteristics of the crystal structure determine its poor conductivity (conductivity is about 10 -9 S / cm, lithium ion diffusion coefficient is about 10 -17 cm 2 / s ), which makes the rate performance of the material, especially the high rate performance, very unsatisfactory, which affects the practical process of the material. How to improve the LiFePO 4 The electrical conductivity, thus improving its electrochemical performance has become a research hotspot; on the other hand, although LiFePO 4 The theoretical density is higher (3.6g / cm 3 ), but in order to improve the electronic conductivity of the material, it is necessary to add conductive carbon, so that its tap density is significantly reduced. In fact, industrialized LiFePO 4 Generally only 1.0g / cm 3 Left and right, resulting in low energy density, making the battery too large to be portable
If the diffusion rate of lithium ions does not reach the rate required for electron migration, the migration of electrons will be limited, which is not conducive to the high rate performance of the material, such as [J] Yuan LXetal Energy&Environmental Science4(2)269-2842011

Method used

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  • Spherical LiFePO4/(C+La2/3-xLi3xTiO3) composite anode material and preparation method thereof
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  • Spherical LiFePO4/(C+La2/3-xLi3xTiO3) composite anode material and preparation method thereof

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Experimental program
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Embodiment 1

[0031] 1.03g LiCO 3 , 1.85g (NH 4 ) 2 HPO 4 , 2.69g citric acid and 5.66g Fe(NO 3 ) 3 9H 2 O mix well, make 70ml aqueous solution, add 0.11g La 0.47 Li 0.60 TiO 3 Mix evenly, then add 1.05g of glycine and mix evenly to obtain a mixed solution, then transfer it to a 100mL lined autoclave, seal it, react with water heat at 190°C for 3.5h, cool, and remove it after the temperature of the reactor drops to room temperature. Solvent to obtain the lithium iron phosphate precursor; after mixing the lithium iron phosphate precursor and 0.44g sucrose in deionized water evenly, stirring and drying at 60°C to obtain the mixture, and then calcining the mixture at 680°C for 8h in an Ar atmosphere, naturally Spherical LiFePO was obtained after cooling 4 / (C+La 0.47 Li 0.60 TiO 3 ) composite cathode material.

[0032] Spherical LiFePO 4 / (C+La 0.47 Li 0.6 TiO 3 ) electronic conductivity from the pure phase of 10-9 S / cm increased to 10 -1 On the order of S / cm, the diffusion r...

Embodiment 2

[0036] 1.17g LiOH·H 2 O, 3.22g NH 4 h 2 PO 4 , 5.38g citric acid and 11.31g Fe(NO 3 ) 3 9H 2 O mixed evenly, made into 70ml aqueous solution, added 2ml of ammonia water with a concentration of 14mol / L and mixed evenly to obtain a mixed solution, then transferred the mixed solution into a 100mL lined autoclave, sealed, and hydrothermally reacted at 180°C for 6h, Cooling, remove the solvent after the reaction kettle temperature is down to room temperature, obtain the lithium iron phosphate precursor; The lithium iron phosphate precursor is mixed with 1.33g citric acid and 0.11g La 0.56 Li 0.33 TiO 3 After mixing evenly in ethanol, stir and dry at 60°C to obtain the mixture, then calcinate the mixture at 700°C for 10 h in an Ar atmosphere, and obtain spherical LiFePO after natural cooling. 4 / (C+La 0.56 Li 0.33 TiO 3 ) composite cathode material.

[0037] image 3 For spherical LiFePO 4 Precursor, Figure 4 For spherical LiFePO 4 / (C+La 0.56 Li 0.33 TiO 3 ) SEM...

Embodiment 3

[0039] 2.04g CH 3 COOLi·2H 2 O, 2.64g (NH 4 ) 2 HPO 4 , 2.50g oxalic acid and 1.60g Fe 2 o 3 Mix evenly to make 60ml of aqueous solution, add 1.46g of diethylamine and mix evenly to obtain a mixed solution, then transfer the mixed solution into a 100mL lined high-pressure reactor, seal it, and conduct a hydrothermal reaction at 160°C for 8 hours, cool, and wait for After the temperature of the reactor is lowered to room temperature, the solvent is removed to obtain a lithium iron phosphate precursor; the lithium iron phosphate precursor is heated in Ar / H 2 Atmosphere (Ar volume ratio is 90%, H 2 Calcined at 650 °C for 8 h in a volume ratio of 10%, and obtained spherical LiFePO after natural cooling 4 Cathode material; spherical LiFePO 4 Cathode material and 0.79g sucrose and 0.19g La 0.49 Li 0.54 TiO 3 After mixing uniformly in an aqueous solution, stir and dry at 70°C to obtain a mixture, and then place the mixture in Ar / H 2 Atmosphere (Ar volume ratio is 90%, H ...

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Abstract

The invention discloses a spherical LiFePO4 / (C+La2 / 3-xLi3xTiO3) composite anode material. According to the composite material, carbon (C) serves as an electron conductor, and La2 / 3-xLi3xTiO3 serving as a fast lithium ion conductor is uniformly mixed and coated on the surface of spherical LiFePO4 so as to form a mixed conductor layer. The mixed conductor layer not only can conduct electrons and lithium ions, but also can prevent an electrolyte from corroding an active material and inhibit Fe from dissolving, so that the improvement on the electrochemical performance of the material is facilitated. The spherical LiFePO4 / (C+La2 / 3-xLi3xTiO3) composite anode material disclosed by the invention has high conductivity and lithium ion diffusion rate, excellent high-magnification performance and high tap density, and is applicable to power type lithium-ion batteries; and the preparation method is simple, feasible, clean and pollution-free, is low in cost and is applicable to industrial scale production.

Description

technical field [0001] The invention belongs to the field of preparation of lithium-ion battery cathode materials, in particular to a spherical LiFePO 4 / (C+La 2 / 3-x Li 3x TiO 3 ) composite cathode material and its preparation method. Background technique [0002] Lithium-ion batteries have become a global research and development hotspot because of their high energy density, low self-discharge rate, no memory effect, long cycle life, low cost and no pollution to the environment. At the same time, the demand for power in the electronics industry, IT industry, communication industry and other fields has soared. Lithium-ion batteries have become portable electrical appliances and The first choice for power supply of electronic instruments. Lithium-ion battery cathode materials account for about 40% of the cost of lithium-ion batteries, and are an important factor determining the cost and electrochemical performance of lithium-ion batteries. focus. However, the most stud...

Claims

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Application Information

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IPC IPC(8): H01M4/04H01M4/58C01B25/45B01J19/00B22F1/02
CPCY02E60/12Y02E60/10
Inventor 王先友舒洪波付艳青杨秀康陈曼芳白艳松易欣胡海郭海鹏谭金黎吴春鞠博伟
Owner XIANGTAN UNIV
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