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Multiple ions co-doped lithium iron phosphate material and preparation method thereof

A lithium iron phosphate and co-doping technology is applied in the field of multi-ion co-doped lithium iron phosphate materials and the preparation thereof, and can solve the problem that the uniform distribution of doping elements cannot be guaranteed, and the olivine-type crystal system structural variation , reduce the electrical properties of materials, etc., to achieve the effects of superior electrochemical performance, improved rate discharge performance, and improved discharge potential platform

Inactive Publication Date: 2015-12-16
WUXI JIABANG ELECTRIC POWER PIPE FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patent has mostly modified lithium iron phosphate by doping, both of them combine the dopant with the main element through simple raw material mixing, ball milling, and roasting. The uniformity of distribution in the material and its occupancy in the lithium iron phosphate lattice can easily lead to a change in the olivine crystal system structure of lithium iron phosphate, resulting in impurity phases, reducing the electrical properties of the material, but failing to achieve improvement. effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Molar ratio (1-y): y, where 0.001≤y≤0.1 Weigh ferrous oxalate and ammonium vanadate into 20L deionized water, and configure a mixture with a total metal ion concentration of 0.07mol / L Solution A; Weigh ammonium dihydrogen phosphate and add it to 0.2L deionized water to make solution B with a concentration of 3mol / L; prepare an ammonia solution with a concentration of 8mol / L; pump the mixed solution A and solution B into the reaction kettle, Control the reaction temperature to 60°C, the stirring speed to 1200rpm, adjust the pH to 2.5 with ammonia water, react for 1.5h, then filter the reaction liquid, wash, and dry to obtain V-doped iron phosphate Fe containing crystal water 0.96 V 0.04 PO 4 2H 2 O.

[0039] (2) Fe obtained in step (1) 0.96 V 0.04 PO 4 2H 2 O was raised from room temperature to 400°C at a heating rate of 5°C / min for 8 hours, and the temperature was naturally lowered to obtain V-doped iron phosphate Fe without crystal water. 0.96 V 0.04 PO 4...

Embodiment 2

[0043] (1) Molar ratio (1-y): y, where 0.001≤y≤0.1 Weigh ferrous oxalate and ammonium vanadate into 20L deionized water, and configure a mixture with a total metal ion concentration of 0.1mol / L Solution A; Weigh ammonium dihydrogen phosphate and add it to 0.2L deionized water to make solution B with a concentration of 5mol / L; prepare an ammonia solution with a concentration of 10mol / L; pump the mixed solution A and solution B into the reaction kettle, Control the reaction temperature to 95°C, the stirring speed to 800rpm, adjust the pH to 3 with ammonia water, react for 0.5h, then filter, wash and dry the reaction liquid to obtain V-doped iron phosphate Fe containing crystal water 0.999 V 0.001 PO 4 2H 2 O.

[0044] (2) Fe obtained in step (1) 0.999 V 0.001 PO 4 2H 2 O was treated from room temperature to 500°C at a heating rate of 1°C / min for 5 hours, and the temperature was naturally lowered to obtain V-doped iron phosphate Fe without crystal water. 0.999 V 0.001 PO...

Embodiment 3

[0048] (1) Molar ratio (1-y): y, where 0.001≤y≤0.1 Weigh ferrous oxalate and ammonium vanadate into 20L deionized water, and configure a mixture with a total metal ion concentration of 0.05mol / L Solution A; weigh ammonium dihydrogen phosphate and add it to 0.2L deionized water to make solution B with a concentration of 0.05mol / L; prepare an ammonia solution with a concentration of 0.5mol / L; pump the mixed solution A and solution B into the reaction kettle In the process, the reaction temperature is controlled at 40°C, the stirring speed is 2500rpm, the pH is adjusted to 2 with ammonia water, and the reaction is carried out for 3 hours, then the reaction liquid is filtered, washed, and dried to obtain V-doped iron phosphate Fe containing crystal water. 0.98 V 0.02 PO 4 2H 2 O.

[0049] (2) Fe obtained in step (1) 0.98 V 0.02 PO 4 2H 2 O was treated from room temperature to 300°C at a heating rate of 2.5°C / min for 10 hours, and the temperature was naturally lowered to obt...

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Abstract

The invention provides a multiple ions co-doped lithium iron phosphate material and a preparation method thereof. This material has a chemical general formula: Li1-zMzFe1-yVy(PO4)1-xFx / C, wherein 0.001< / =x< / =0.1, 0.001< / =y< / =0.1, 0.001< / =z< / =0.1, and M is lithium-doped metal ions. The preparation method includes: preparing vanadium ion doped iron phosphate Fe1-yVyPO4.2H2O containing crystal water, and performing thermal treatment to obtain vanadium doped iron phosphate Fe1-yVyPO4 not containing crystal water; adding a ball-milling medium, allowing ball milling and mixing, performing pre-sintering, performing calcining at high temperature, and performing grinding after cooling to obtain multiple ions co-doped lithium iron phosphate powdered material. The preparation method is simple, energy consumption is low, raw materials are low in price, and industrial production of the material is facilitated.

Description

technical field [0001] The invention relates to the field of lithium ion battery materials, in particular to a multi-ion co-doped lithium iron phosphate material and a preparation method thereof. The material can be used in lithium-ion batteries, supercapacitors and capacitive batteries. Background technique [0002] Since 1997, J.B.Goodnough [J.Electrochem.Soc., 144 (1997) 1188] research group first reported olivine-type LiFePO 4 And since it is used as a cathode material for lithium-ion batteries, because LiFePO 4 It has the characteristics of non-toxicity, stable structure, high specific capacity, long cycle life, low manufacturing cost, good safety performance and environmental friendliness, and is considered to be one of the most promising cathode materials for lithium-ion power batteries. [0003] However, LiFePO 4 The inherently low electronic conductivity and ion conduction rate greatly limit its practical application in the field of lithium-ion power batteries. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45C01B25/26H01M4/58H01G11/50
CPCY02E60/10Y02E60/13
Inventor 徐德生
Owner WUXI JIABANG ELECTRIC POWER PIPE FACTORY
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