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Hydrothermal preparation method of nano lithium iron manganese phosphate anode material

A lithium iron manganese phosphate, cathode material technology, applied in nanotechnology, chemical instruments and methods, phosphorus compounds, etc., can solve the problems of easy decomposition of manganese element, low conductivity, etc., achieve good crystallinity, improve conductivity, and purity. high effect

Active Publication Date: 2014-04-30
XTC NEW ENERGY MATERIALS(XIAMEN) LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But LiMnPO 4 The conductivity is low, and the manganese element is easy to decompose in the electrolyte, etc.

Method used

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  • Hydrothermal preparation method of nano lithium iron manganese phosphate anode material
  • Hydrothermal preparation method of nano lithium iron manganese phosphate anode material
  • Hydrothermal preparation method of nano lithium iron manganese phosphate anode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 2L of deionized water into the sealed reaction kettle, add 6.0mol LiOH·H 2 O and 2.0mol 85%H 3 PO 4 Add to the reaction kettle respectively, add while stirring, and then add concentrated ammonia water with a mass fraction of 25% into the reaction kettle to control the pH value in the reaction kettle within the range of 9 to 10, and seal the reaction kettle. At the same time, the temperature was raised to 180°C, and 0.6mol FeSO 4 ·7H 2 O, 1.38mol MnSO 4 ·H 2 O and 0.02mol Ti (SO 4 ) 2 Add it into 2L of deionized water, stir evenly, pump the solution into the reaction kettle with a high-pressure pump, and control the addition speed so that the temperature in the reaction kettle is within the range of 170-200°C during the addition process. The reaction kettle was heated, and the temperature in the reaction kettle was raised to 200° C. for 10 hours. After cooling, when the reaction kettle is cooled below 60°C, wash the material with deionized water until there i...

Embodiment 2

[0024] Add 2L of deionized water into the sealed reaction kettle, add 6.0mol LiOH·H 2 O and 2.0mol 85%H 3 PO 4 Add to the reaction kettle respectively, add while stirring, and then add concentrated ammonia water with a mass fraction of 25% into the reaction kettle to control the pH value in the reaction kettle within the range of 9 to 10, and seal the reaction kettle. The closed reaction kettle was heated to 180°C at the same time, and 0.99mol FeSO 4 ·7H 2 O, 0.99mol MnSO 4 ·H 2 O and 0.02mol Ti (SO 4 ) 2 Add it into 2L of deionized water, stir evenly, pump the solution into the reaction kettle with a high-pressure pump, and control the addition speed so that the temperature in the reaction kettle is within the range of 170-200°C during the addition process. The reaction kettle was heated, and the temperature in the reaction kettle was raised to 200° C. for 10 hours. After cooling, when the reaction kettle is cooled below 60°C, wash the material with deionized water un...

Embodiment 3

[0027] Add 2L of deionized water into the sealed reaction kettle, add 6.0mol LiOH·H 2 O and 2.0mol 85%H 3 PO 4 Add to the reaction kettle respectively, add while stirring, and then add concentrated ammonia water with a mass fraction of 25% into the reaction kettle to control the pH value in the reaction kettle within the range of 9 to 10, and seal the reaction kettle. The closed reaction kettle was heated to 180°C at the same time, and 0.4mol FeSO4 ·7H 2 O, 1.58mol MnSO 4 ·H 2 O and 0.02mol Ti (SO 4 ) 2 Add it into 2L of deionized water, stir evenly, pump the solution into the reaction kettle with a high-pressure pump, and control the addition speed so that the temperature in the reaction kettle is within the range of 170-200°C during the addition process. The reaction kettle was heated, and the temperature in the reaction kettle was raised to 200° C. for 10 hours. After cooling, when the reaction kettle is cooled below 60°C, wash the material with deionized water until...

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Abstract

The invention discloses a hydrothermal preparation method of a nano lithium iron manganese phosphate anode material. The method comprises the following steps: preparing a precursor, namely mixing a H3PO4 solution and LiOH H2O according to a molar ratio 3:1 of Li:P; adding stronger ammonia water until the pH value is 9-10; raising the temperature to 180 DEG C, adding the solution into deionized water according to a molar ratio 0.99:0.01:1 of (Fe+Mn):Ti:P, pumping the mixed solution into a reaction kettle, and regulating the temperature to be 170-200 DEG C; heating to the temperature of 200 DEG C, and keeping the temperature for 7-10 hours; washing and performing carbon coating; washing until sulfate radical does not exist by using the deionized water when the solution is cooled to 60 DEG C or below, adding a soluble organic matter carbon source, performing spray drying, performing heat treatment for 7-10 hours, and cooling to obtain LiMnxFe0.99-xTi0.01PO4 powder. The process method is simple, controllable, convenient to operate and high in industrialization degree, and the prepared nano lithium iron manganese phosphate material is high in specific energy, stable in performance and good in consistency.

Description

technical field [0001] The invention relates to the preparation technology of the cathode material of lithium ion battery, in particular to a hydrothermal preparation method of the cathode material of nano manganese iron phosphate lithium. Background technique [0002] Lithium iron phosphate (LiFePO 4 ) has the advantages of good safety performance, excellent cycle performance and environmental friendliness, and has abundant raw materials and high specific capacity. However, lithium iron phosphate has problems such as low ion conductivity and electronic conductivity, and insufficient specific energy, which have become key factors restricting the large-scale application of lithium iron phosphate batteries. In recent years, lithium manganese phosphate (LiMnPO) with olivine structure 4 ) material research has achieved great results. Compared to LiFePO 4 , LiMnPO 4 It has the advantages of high discharge voltage and high power density. But LiMnPO 4 The conductivity is low...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58C01B25/45B82Y40/00
CPCB82Y40/00C01B25/45H01M4/5825H01M10/0525Y02E60/10
Inventor 章明钱文连张文新陈惠明王耀南杨金洪
Owner XTC NEW ENERGY MATERIALS(XIAMEN) LTD
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