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Preparation methods of NH4Fe1-xMxPO4 and LiFe1-xMxPO4/C materials

A technology of nh4fe1-xmxpo4, CH3COO, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve dangerous and cumbersome problems

Active Publication Date: 2017-03-08
ENERGY RES INST OF SHANDONG ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The hydrothermal method has high requirements on the reaction equipment and needs to be operated in a high-temperature and high-pressure reactor, which is relatively cumbersome and dangerous

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Weigh Fe(NO 3 ) mass is 16.406g, phosphoric acid mass is 11.984g, Mn(NO 3 ) 2 The mass is 10.245g, the mass of citric acid is 0.09g, and deionized water is added to make a mixed solution with a concentration of 0.2 mol / liter; the concentration of ammonia water is configured to be 2 mol / liter, and the flow pump is used to continuously input to a container with a stirrer. Quantitative deionized water and N 2 In the sealed reaction kettle, control the temperature of the reaction solution in the reaction kettle to 20°C, make the pH of the reaction solution in the reaction kettle = 5, stir and react for 1 hour, unload after the reaction is completed, wash, dry, and heat treatment to finally obtain flakes NH 4 Fe 0.4 mn 0.6 PO 4 Precursor.

[0045] According to the stoichiometric ratio Li:(Fe+Mn):P=1:1:1 (molar ratio), the lithium source, NH 4 Fe 0.4 m 0.6 PO 4 Precursor, sucrose and deionized water ball mill are mixed evenly, dried and placed in a tube furnace fil...

Embodiment 2

[0047] Weigh Fe(NO 3 ) mass is 16.406g, phosphoric acid mass is 11.984g, Co(NO 3 ) 2 The mass is 8.732g, the mass of citric acid is 0.09g, and deionized water is added to make a mixed solution with a concentration of 0.2 mol / liter; the concentration of ammonia water is configured to be 2 mol / liter, and a flow pump is used to continuously input it into a container with a stirrer. Quantitative deionized water and N 2 In the sealed reaction kettle, control the temperature of the reaction solution in the reaction kettle to 20°C, make the pH of the reaction solution in the reaction kettle = 7, stir and react for 1 hour, unload after the reaction is completed, wash, dry, and heat treatment to finally obtain flakes NH 4 Fe 0.4 co 0.6 PO 4 Precursor.

[0048] According to the stoichiometric ratio Li:(Fe+Co):P=1:1:1 (molar ratio), the lithium source, NH 4 Fe 0.4 co 0.6 PO 4 Precursor, sucrose and deionized water ball mill are mixed evenly, dried and placed in a tube furnace ...

Embodiment 3

[0050] Weigh Fe(NO 3 ) quality is 16.406g, phosphoric acid quality is 11.984g, Ni(NO 3 ) 2 The mass is 8.315g, the mass of citric acid is 0.09g, and deionized water is added to make a mixed solution with a concentration of 1.0 mol / liter; the concentration of ammonia water is configured to be 5 mol / liter, and the flow pump is used to continuously input to a container with a stirrer respectively. Quantitative deionized water and N 2 In the sealed reaction kettle, control the temperature of the reaction solution in the reaction kettle to 50°C, make the pH of the reaction solution in the reaction kettle = 10, stir and react for 6 hours, unload after the reaction is completed, wash, dry, and heat treatment to finally obtain flakes NH 4 Fe 0.4 Ni 0.6 PO 4 Precursor.

[0051] According to the stoichiometric ratio Li:(Fe+Ni):P=1.05:1:1 (molar ratio), the lithium source, NH 4 Fe 0.4 mn 0.4 Ni 0.2 PO 4 Precursor, sucrose and deionized water ball mill are mixed evenly, dried ...

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Abstract

The invention provides a preparation method of NH4Fe1-xMxPO4 and LiFe1-xMxPO4/C materials. The preparation method of the LiFe1-xMxPO4/C material includes preparing a phosphorus source compound, a ferrous iron compound, a bivalent M metallic salt compound (M=Ni, Co and Mn) and a reducing agent into a mixture water solution, enabling the mixture water solution to react with an ammonia water solution to synthesize a sheet-shaped NH4Fe1-xMxPO4 precursor, and performing lithium doping and high-temperature heat treatment to obtain the LiFe1-xMxPO4/C material. The LiFe1-xMxPO4/C material prepared according to the preparation method has the advantages of high energy density, good cycle performance and high rate capability and is suitable for the application field of lithium-ion power batteries. The preparation method has the advantages of simple steps, convenience in operation and high practicality.

Description

technical field [0001] The invention belongs to the technical field of energy materials, in particular to a kind of NH 4 Fe 1-x m x PO 4 and LiFe 1-x m x PO 4 / C material preparation method. Background technique [0002] Since its inception, lithium-ion batteries have been favored by people because of their advantages such as high energy density, stable discharge voltage, and long working life. They are widely used in portable energy storage tools, especially in recent years. The field of new energy vehicles. As an important part of lithium-ion batteries, the choice of cathode materials directly affects the electrochemical performance of lithium-ion batteries. [0003] At present, the anode materials of lithium-ion batteries that have been industrialized and commercially used are mainly lithium cobaltate, lithium manganate and lithium iron phosphate, among which lithium cobaltate is highly toxic, expensive, and has certain safety problems; the spinel structure Lithi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/36H01M4/58H01M4/62H01M10/0525
CPCC01B25/45C01B25/451C01P2004/62C01P2006/40H01M4/366H01M4/5825H01M4/625H01M10/0525Y02E60/10
Inventor 秦显忠杨改蔡飞鹏高剑应皆荣
Owner ENERGY RES INST OF SHANDONG ACAD OF SCI
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