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Multi-ion co-doping lithium iron phosphate material and preparation method thereof

A lithium iron phosphate and co-doping technology, which is applied in the field of multi-ion co-doped lithium iron phosphate materials and its preparation, can solve the problem of inability to ensure the uniform distribution of doping elements and occupancy, and the variation of olivine crystal system structure , reduce the electrical properties of materials and other issues, and achieve the effects of superior electrochemical performance, improved rate discharge performance, and improved discharge potential platform

Inactive Publication Date: 2016-08-10
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 multi-ion co-doping lithium iron phosphate material and a preparation method thereof. The chemical formula of the multi-ion co-doping lithium iron phosphate material is Li<1-z>M<2>Fe<1-y>V<y>(PO<4>)<1-x>F<x> / C, wherein x is more than or equal to 0.001 but less than or equal to 0.1, y is more than or equal to 0.001 but less than or equal to 0.1, z is more than or equal to 0.001 but less than or equal to 0.1, and M is lithium position doping metal ion. The preparation method comprises the following steps of firstly, preparing vanadium ion doping iron phosphate Fe<1-y>V<y>PO<4>.2H<2>O containing crystal water; secondly, obtaining vanadium doping iron phosphate Fe<1-y>V<y>PO<4> which does not contain the crystal water by thermal processing; and finally, adding a ball-milling medium, carrying out ball-milling mixing, carrying out pre-sintering and then calcination in a high temperature, and cooling and grinding the mixture to obtain the multi-ion co-doping lithium iron phosphate powder material. The method is simple in process, energy consumption is relatively low, the raw material is low in cost, and industrial production at a large scale 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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IPC IPC(8): H01M4/36H01M4/58
CPCH01M4/364H01M4/5805Y02E60/10
Inventor 徐德生
Owner WUXI JIABANG ELECTRIC POWER PIPE FACTORY
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