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A method of preparing multi-site synergistically doped lifepo4/c by ultrasonic spraying of phosphate fertilizer products

A phosphate fertilizer product and ultrasonic technology, applied in the field of electrochemical power supply material preparation, can solve problems such as lack of performance, large particle size of materials, unfavorable mass production, etc., and achieve the effect of increasing added value, good dispersibility, and good cycle performance

Active Publication Date: 2018-06-15
宜春鑫合锂电材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, the solid-phase method and the carbothermal reduction method are simple and easy to operate, and can be used in industrial production. However, the synthesized materials have large particle sizes and lack performance. Other synthetic methods are not conducive to industrial mass production.

Method used

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  • A method of preparing multi-site synergistically doped lifepo4/c by ultrasonic spraying of phosphate fertilizer products
  • A method of preparing multi-site synergistically doped lifepo4/c by ultrasonic spraying of phosphate fertilizer products
  • A method of preparing multi-site synergistically doped lifepo4/c by ultrasonic spraying of phosphate fertilizer products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Oxygen doping

[0038] A preparation of multi-position synergistically doped LiFePO by ultrasonic spraying of phosphate fertilizer products 4 / C method, the steps are as follows:

[0039] (1) Primary mixing of parent material and dopant

[0040] Mix lithium hydroxide as raw material for lithium, ferric nitrate as raw material for iron, ammonium dihydrogen phosphate as raw material for phosphorus, and ammonium sulfide as doping source for oxygen at a molar ratio of 1:1:1:0.15, add water-soluble starch, and the mass of water-soluble starch It is 10% of the quality of ferric nitrate, with deionized water as a solvent, fully stirred in a stirring device (rotating speed=200 rev / min) until the raw materials are all dissolved, filtered to obtain a precursor solution, the concentration of lithium ions in the precursor solution is 1mol / L.

[0041] (2) Ultrasonic spray

[0042] The prepared precursor solution is sent into the ultrasonic nebulizer with an inert gas a...

Embodiment 2

[0047] Example 2 Oxygen site doping

[0048] A preparation of multi-position synergistically doped LiFePO by ultrasonic spraying of phosphate fertilizer products 4 / C method, the steps are as follows:

[0049] (1) Primary mixing of parent material and dopant

[0050] Mix lithium acetate as raw material for lithium, ferric nitrate as raw material for iron, ammonium dihydrogen phosphate as raw material for phosphorus, and ammonium fluoride as doping source for oxygen at a molar ratio of 1:1:1:0.4, add glucose, and the mass of glucose is the mass of ferric nitrate Using deionized water as a solvent, fully stir in a stirring device (rotating speed = 200 rpm) until all the raw materials are dissolved, filter to obtain a precursor solution, the concentration of lithium ions in the precursor solution is 1mol / L.

[0051] (2) Ultrasonic spray

[0052] The prepared precursor solution is sent into the ultrasonic nebulizer with an inert gas as the carrier gas through an air compression...

Embodiment 3

[0057] Example 3 Lithium and oxygen doping

[0058] A preparation of multi-position synergistically doped LiFePO by ultrasonic spraying of phosphate fertilizer products 4 / C method, the steps are as follows:

[0059] (1) Primary mixing of parent material and dopant

[0060] The lithium-site raw material lithium oxalate, the iron-site raw material iron nitrate, the phosphorus-site raw material ammonium dihydrogen phosphate, the lithium-site doping source potassium dihydrogen phosphate, and the oxygen-site doping source ammonium sulfide in a molar ratio of 0.49:1:0.98:0.02:0.3 Mixing, adding sucrose, the quality of sucrose is 10% of the mass of ferric nitrate, using deionized water as solvent, fully stirring in a stirring device (speed = 200 rpm) until all the raw materials are dissolved, filtering to obtain a precursor solution, The lithium ion concentration in the precursor solution was 0.98mol / L.

[0061] (2) Ultrasonic spray

[0062] The prepared precursor solution is se...

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Abstract

The invention belongs to the technical field of electrochemical power source materials and discloses a method of adopting phosphorus fertilizer product for ultrasonic spraying to prepare multi-position collaborative doped LiFePO4 / C. Raw materials of the multibit collaborative doped LiFePO4 / C are from the phosphorus fertilizer product and byproducts and include Li, P, Fe, doped element cations K, Na, Ca and Mg and anions S and F. The multibit collaborative doped lithium iron phosphate material is marked as Li1-alpha X alpha Fe1-beta Y beta PO4-gamma Z gamma / C, X refers to lithium position doping, Y refers to iron position doping, Z refers to oxygen position doping, 0< / =alpha< / =0.05, 0< / =beta< / =0.05, and 0< / =gamma< / =2. Collaborative doping of lithium position, iron position and oxygen position is realized, and doping amount is adjustable; compared with single doping, doping materials are extensive in source, and the material is better in performance. The multi-position collaborative doped LiFePO4 / C material is uniform in grain diameter and excellent in electrochemical performance.

Description

technical field [0001] The invention relates to the technical field of preparation of electrochemical power source materials, in particular to a method of preparing multi-position synergistically doped LiFePO by using phosphate fertilizer products as raw materials and adopting ultrasonic spray method 4 / C lithium-ion battery cathode material method. Background technique [0002] Phosphate fertilizer is a pillar industry related to agriculture in my country. In 2015, the national phosphate fertilizer output was nearly 20 million tons, while the national fertilizer application was about 8 million to 9 million tons. The production capacity has more than doubled the domestic market demand, resulting in a large backlog of phosphate fertilizers. At the same time, domestic phosphorus The trend of resource depletion has intensified, and the state has issued a series of policies to restrict the development of phosphate rock resources, resulting in expensive raw materials for the produ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M4/62H01M10/0525
CPCH01M4/364H01M4/5825H01M4/583H01M4/625H01M10/0525Y02E60/10
Inventor 陈连清赵轩郭勇
Owner 宜春鑫合锂电材料有限公司
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