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Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon

A graphitized carbon and lithium iron phosphate technology, applied in battery electrodes, lithium batteries, structural parts, etc., can solve problems such as increased cost, poor carbon conductivity, and difficulty in improving the conductivity of lithium iron phosphate, and achieve particle size distribution Uniform, excellent room temperature rate performance and cycle performance, high purity effect

Inactive Publication Date: 2015-07-15
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the method of increasing the conductivity through coating doping alone, or modifying the lithium transport channel can no longer meet the requirements of power batteries for high-current charge and discharge of positive electrode materials.
The currently used lithium iron phosphate materials are generally sintered at high temperature, which increases the cost to a certain extent, and the carbon produced by the carbonization of organic matter has poor electrical conductivity, so it is difficult to further improve the conductivity of lithium iron phosphate

Method used

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  • Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon
  • Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon
  • Method for preparing lithium iron phosphate positive electrode material coated by home position graphitization carbon

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Weigh 24.55g ferrocene, 10.30g35% formaldehyde solution, 4.91g anhydrous ZnCl 2 Add it into a 500mL three-necked flask, heat it in an oil bath at 120°C for 10 hours, and keep it under vigorous mechanical stirring. After the reaction, cool it down to room temperature naturally, and wash it three times with a mixed solvent of benzene and dichloromethane with a volume ratio of 1:1. , washed with deionized water until the washing solution was colorless, and the obtained black solid was vacuum-dried at 100° C. for 12 hours. Weigh 3.8519g of dried black powder, 0.7192gLi 2 CO 3 , 2.2195gNH 4 h 2 PO 4 Add it into a 100mL agate ball mill jar, control the ball-to-material ratio to 5:1, pour 15mL of acetone with a purity of 99.9% as a dispersion medium, and mill at 220r / min for 5 hours, and use an additional 10mL of a pure material with a purity of 99.9% Disperse with acetone, pour it into a petri dish, and dry it in vacuum at 80°C for 12 hours. Grind the dried sample, put i...

Embodiment 2

[0031] Weigh 24.55g ferrocene, 13.215g40% acetaldehyde solution, 4.91g anhydrous ZnCl 2, 3.5514g of 37% concentrated hydrochloric acid was added to a 500mL three-necked flask, heated by an oil bath at 160°C for 8 hours, accompanied by vigorous mechanical stirring during the heat preservation process, and naturally cooled to room temperature after the reaction was completed. The mixed solvent of methyl chloride was washed three times, and then washed with deionized water until the washing liquid was colorless, and the obtained black solid was vacuum-dried at 100° C. for 12 hours. Weigh the dried black powder 2.0623g, 0.8291gFe 2 o 3 , 0.7891gLi 2 CO 3 , 2.3912gNH 4 h 2 PO 4 , 0.1717gMnAc 2 4H 2 O was added to a 100mL agate ball mill jar, the ratio of balls to materials was 10:1, 15mL of acetone with a purity of 99.9% was poured into it as a dispersion medium, and ball milled at 200r / min for 8 hours, and an additional 10mL of acetone with a purity of 99.9% was used for t...

Embodiment 3

[0033] Weigh 24.55g ferrocene, 12.7344g benzaldehyde, 4.91g anhydrous ZnCl 2 , 5.3270g of 37% concentrated hydrochloric acid was added to a 500mL three-necked flask, heated in an oil bath at 170°C for 6 hours, accompanied by vigorous mechanical stirring during the heat preservation process, and naturally cooled to room temperature after the reaction, using benzene and dihydrogen at a volume ratio of 1:1 The mixed solvent of methyl chloride was washed three times, and then washed with deionized water until the washing liquid was colorless, and the obtained black solid was vacuum-dried at 100° C. for 12 hours. Weigh the dried black powder 1.5995g, 2.2042g FeC 2 o 4 , 2.5569g LiH 2 PO 4 , 0.3508gNiAc 2 4H 2 O was added to a 100mL agate ball mill jar, the ratio of the ball to material was 15:1, poured 15mL of acetone with a purity of 99.9% as the dispersion medium, and milled at 150r / min for 9 hours, and used an additional 10mL of the viscous material with a purity of 99.9% ...

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Abstract

The invention discloses a method for preparing a lithium iron phosphate positive electrode material coated by home position graphitization carbon. The method includes the following steps that ferrocene, aldehyde, and zinc chloride or / and concentrated hydrochloric acid are added into a flask according to a certain proportion; heating is carried out for 1-10 hours in oil bath at the temperature of 120-180 DEG C, stirring and polymerization are conducted, and after washing, the prepared poly-ferrocene is used as an iron source; a lithium source, the iron source, a phosphate radical source and a doping source of a certain proportion are added, the mixture is mixed for 3-9 hours in a ball-milling mode according to the certain proportion, after the mixture is fully dried in a vacuum mode under 80 DEG C, thermal insulation is conducted for 1-12 hours under 250-400 DEG C, argon serves as the protective atmosphere, cooling is carried out so that an indoor temperature can be achieved along with a furnace, and lithium iron phosphate coated by the home position graphitization carbon is obtained. According to the method for preparing the lithium iron phosphate positive electrode material coated by the home position graphitization carbon, the grain diameter d50 of prepared lithium iron phosphate powder is smaller than or equal to 100nm, and excellent rate performance and cycle performance are achieved.

Description

technical field [0001] The invention relates to a preparation method of nano-lithium iron phosphate, in particular to a preparation method of an in-situ graphitized carbon-coated lithium iron phosphate cathode material. Background technique [0002] The lithium iron phosphate cathode material was first discovered by the Goodenough group in 1997. The material consists of FeO 6 Octahedron and PO 4 The tetrahedrons are connected together to form a stable olivine structure skeleton. Lithium ions can be released and inserted freely from the b-axis direction. There will be no large lattice distortion during the movement of lithium ions, and it has very good safety. Therefore, it is currently The most promising cathode material for power batteries. LiFePO 4 It has a high theoretical specific capacity of 170mAh / g, a high energy density of 550Wh / Kg, good cycle stability, environmental friendliness, and low cost. It is widely favored and put into a lot of research. [0003] Howev...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M4/1397
CPCH01M4/366H01M4/5825H01M4/625H01M10/052Y02E60/10
Inventor 张建新姚斌丁昭郡冯小钰路婷婷
Owner SHANDONG UNIV