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A method for controllable preparation of sodium manganese fluorophosphate cathode material

A technology for preparing sodium manganese fluorophosphate and obtaining sodium manganese fluorophosphate, applied in battery electrodes, structural parts, electrical components, etc., can solve the unreported Na2MnPO morphology controllable preparation technology, the particles are not suitable for battery materials, and unreported Electrochemical performance and other issues, to achieve the effect of improving electrochemical performance, increasing synthesis efficiency, and good crystallinity

Active Publication Date: 2021-07-09
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of Na by hydrothermal method 2 PPML 4 F Rarely reported, only Bagtache et al. (Materials Science in Semiconductor Processing 2016, 51:1-7) used the hydrothermal method to synthesize "long oval" Na 2 PPML 4 f
However, even though it took 5 days, its XRD showed that the crystallinity of the product was not very good, and the synthesized Na 2 PPML 4 The size of F long oval particles is as high as 40-60μm, and for Na with very low conductivity 2 PPML 4 For F, particles that are too coarse will not be suitable for use in battery materials
In fact, the report only puts Na 2 PPML 4 F is used for the test of photoelectric performance, and its electrochemical performance is not reported
In addition, this study did not report Na 2 PPML 4 The morphology controllable preparation technology of F
Therefore, there is no hydrothermal method to prepare Na with different morphology. 2 PPML 4 F controllable preparation technology reports, and no use of hydrothermal method to control Na 2 PPML 4 A report on the crystallinity and morphology of F to enhance the electrochemical performance of materials

Method used

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  • A method for controllable preparation of sodium manganese fluorophosphate cathode material
  • A method for controllable preparation of sodium manganese fluorophosphate cathode material
  • A method for controllable preparation of sodium manganese fluorophosphate cathode material

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Molar ratio Na:Mn:PO 4 : F=6.5: 1: 1: 2.5 Weigh sodium fluoride, sodium hydroxide, phosphoric acid and manganese nitrate, take deionized water as solvent, stir at room temperature, then add ascorbic acid (mass ratio is sodium manganese fluorophosphate: Ascorbic acid=2:1), continue stirring to form a solution or suspension;

[0032]b. Seal the solution or suspension prepared in step a in an autoclave, place it in a blast drying oven at 280°C for 6 hours, and then cool it naturally to room temperature;

[0033] c. Take out the product in the reaction kettle, separate the solid from the liquid, collect the solid, wash it three times with deionized water, then dry it in a blast drying oven at 80°C, and cool it to room temperature to obtain Na 2 PPML 4 F cathode material.

Embodiment 2

[0035] a. Molar ratio Na:Mn:PO 4 : F=6.5: 1: 1: 2.5 Weigh sodium hydroxide, sodium dihydrogen phosphate, manganese nitrate and ammonium fluoride, take deionized water as solvent, stir at room temperature, then add tartaric acid (mass ratio is fluorophosphoric acid Sodium manganese: tartaric acid=2: 0.9), continue stirring to form a solution or suspension;

[0036] b. Seal the solution or suspension prepared in step a in an autoclave, place it in a blast drying oven at 220°C for 12 hours, and then cool it naturally to room temperature;

[0037] c. Take out the product in the reaction kettle, separate the solid from the liquid, collect the solid, wash it three times with deionized water, then dry it in a blast drying oven at 60°C, and cool it to room temperature to obtain Na 2 PPML 4 F cathode material.

Embodiment 3

[0039] a. Molar ratio Na:Mn:PO 4 : F=6.5: 1: 1: 2.5 Weigh sodium fluoride, sodium hydroxide, ammonium dihydrogen phosphate and manganese acetate, take deionized water as solvent, stir at room temperature, then add citric acid (mass ratio is fluorine Sodium manganese phosphate: citric acid=2: 1), continue stirring to form a solution or suspension;

[0040] b. Seal the solution or suspension prepared in step a in an autoclave, place it in a blast drying oven at 180°C for 72 hours, and then cool it naturally to room temperature;

[0041] c. Take out the product in the reaction kettle, separate the solid from the liquid, collect the solid, wash it three times with deionized water, then dry it in a blast drying oven at 100°C, and cool it to room temperature to obtain Na 2 PPML 4 F cathode material.

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Abstract

The invention discloses a controllable method for preparing sodium manganese fluorophosphate positive electrode material. The sodium source, manganese source, phosphoric acid source, fluorine source and chelating agent are dissolved in deionized water to form a solution or suspension according to the stoichiometric ratio. Seal it in a high-pressure reactor and heat the reaction, cool to room temperature, take out the product, separate the solid from the liquid, collect the solid, wash it with deionized water several times, and dry it to obtain the sodium manganese fluorophosphate positive electrode material. The method of the present invention regulates the nucleation conditions and crystal growth direction of the sodium manganese fluorophosphate crystal grains by adding a chelating agent and process parameters, changes the morphology of the sodium manganese fluorophosphate, improves the electrochemical performance of the sodium manganese fluorophosphate material, and greatly Shorten synthesis time, improve production efficiency and reduce energy consumption.

Description

technical field [0001] The invention belongs to the field of electrode materials and the field of electrochemical energy storage, and relates to sodium manganese fluorophosphate (Na 2 PPML 4 The preparation of F) specifically relates to a method for controllable preparation of sodium manganese fluorophosphate cathode material. Background technique [0002] In recent years, with the rapid development of new energy (solar, wind, etc.) power generation and grid energy storage technologies, the demand for secondary batteries has surged. Lithium-ion batteries have been widely used in various electronic devices due to their excellent performance. However, the economically recoverable reserves of lithium are very limited, and it is difficult to meet the needs of long-term development in the future. Therefore, sodium, which has similar physical and chemical properties to lithium and is cheap, has attracted widespread attention. Sodium and lithium belong to the same main group. Com...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/58H01M10/054
CPCH01M4/5825H01M10/054Y02E60/10
Inventor 伍凌胡勇钟胜奎廖桂祥张晓萍刘洁群
Owner SUZHOU UNIV
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