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Preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material

A porous sodium ferrous fluorophosphate, three-dimensional ordered technology, applied in the field of preparation of three-dimensional ordered macroporous sodium ferrous fluorophosphate materials, can solve the problems of 3DOMNa preparation and electrochemical performance research that have not been reported in relevant literature, and achieve The effect of reducing ion diffusion distance, improving cycle performance, and large charge-discharge specific capacity

Active Publication Date: 2022-05-13
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no related literature reporting 3DOMNa 2 FePO 4 Preparation and electrochemical performance of F

Method used

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  • Preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material
  • Preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material
  • Preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) 0.01g of sodium dodecylsulfonate is dissolved in 250ml of deionized water, then 35g of PMMA monomer and 0.28g of potassium persulfate are added to the above solution, under the condition of feeding nitrogen, 70 Stir at reflux for 2.5h. The obtained PMMA emulsion was dried at 50° C., and the microspheres self-assembled to obtain a colloidal crystal template.

[0027] (2) With ferric nitrate nonahydrate, sodium fluoride, sodium nitrate and phosphoric acid as raw materials, the molar ratio of substances Na:Fe:P:F is 2:1:1:1 to weigh raw materials; first weigh 8.08g nine Ferric nitrate hydrate, 3.5g antioxidant ascorbic acid, 2.31g phosphoric acid (mass percentage is 85%) add 25ml deionized water and dissolve in the beaker to obtain solution A; Then take by weighing 1.7g sodium nitrate and 0.84g sodium fluoride plus 25ml deionized Dissolve water in a beaker to obtain solution B; finally, stir and mix solution A and solution B evenly to obtain a concentration of 0.4mol ...

Embodiment 2

[0033] (1) is the same as example 1 step (1).

[0034] (2) Ferric nitrate nonahydrate, sodium fluoride, sodium hydroxide, and ammonium dihydrogen phosphate are used as raw materials, and the raw materials are weighed according to the molar ratio of substances Na:Fe:P:F of 2:1:1:2. First weigh 4.04g ferric nitrate nonahydrate, 2.10g citric acid, 1.15g ammonium dihydrogen phosphate and 25ml deionized water and dissolve in a beaker to obtain solution A, then weigh 0.84g sodium fluoride and 25ml deionized water and dissolve in a beaker Obtain solution B, and finally mix solution A and solution B evenly to obtain a concentration of 0.2mol L -1 Sol

[0035] (3) Add the colloidal crystal template prepared in step (1) to the sol obtained in step (2), fully soak for 5-6 hours, and then remove excess sol by suction filtration. The obtained template sol complex was dried at 50°C for use.

[0036] (4) Place the template filled in step (3) in an atmosphere furnace, pass in argon gas, ra...

Embodiment 3

[0040] (1) is the same as example 1 step (1).

[0041] (2) Take ferrous sulfate heptahydrate, sodium fluoride, sodium acetate, and phosphoric acid as raw materials, and weigh the raw materials according to the molar ratio of substances Na:Fe:P:F of 2:1:1:1, first weigh 4.86g Ferrous sulfate heptahydrate, 0.123g of antioxidant ascorbic acid, 2.018g of phosphoric acid plus 25ml of deionized water were dissolved in a beaker to obtain solution A, and then 2.382g of sodium acetate and 0.735g of sodium fluoride were added and dissolved in 25ml of deionized water in a beaker to obtain Solution B, and finally mix solution A and solution B evenly to obtain a sol concentration of 0.35mol L -1 ;

[0042] (3) Add the colloidal crystal mold prepared in step (1) to the sol obtained in step (2) and immerse for 5-6 hours. After fully filling, remove the excess sol by suction filtration, and then compound the obtained template sol The material was dried at 50°C until use.

[0043] (4) Place...

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Abstract

The invention relates to a preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material. Based on the colloidal crystal template method, different concentrations of Na 2 FePO 4 The F precursor sol fills the template, and during the sintering process, a three-dimensional ordered macroporous Na 2 FePO 4 For material F, the diameter of the macropore is about 150-180nm, the thickness of the pore wall is about 30-50nm, and the channels are uniform and orderly. The method is simple and the process is simple. As the positive electrode material of the sodium ion battery, due to its special porous structure, the contact area between the electrolyte and the active material can be increased, and the volume change in the process of sodium ion intercalation and extraction can be alleviated, which is conducive to improving the cycle performance and Rate performance, electrochemical tests show that at a current density of 0.1C, the first discharge capacity can reach 107mAh g ‑1 . At 0.5C, its specific capacity can still maintain 85.5% after 500 cycles.

Description

technical field [0001] The invention relates to a preparation method of a three-dimensional ordered macroporous sodium ferrous fluorophosphate material. The invention belongs to the application field of inorganic nanometer materials. Background technique [0002] As a representative of energy storage technology, lithium-ion batteries have been widely used in various portable batteries due to their high energy density and high power density, high output voltage, long cycle life, no memory effect, small size, and light weight. In electronic equipment, and with the gradual popularization of new energy vehicles, human demand for lithium resources will increase significantly. However, the lithium resources on the earth are very limited, and the abundance in the crust is only 20mg kg -1 , and the distribution is uneven and the price is high, which seriously restricts the development of lithium-ion batteries to large-scale energy storage applications. In contrast, sodium and lit...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/455H01M4/58H01M10/054B82Y40/00
CPCH01M4/5825H01M10/054B82Y40/00C01B25/455H01M2004/028H01M2004/021C01P2006/40C01P2002/72C01P2004/03Y02E60/10
Inventor 蔡舒沈凯尔凌瑞谢东篱孙佳月韦洁玲
Owner TIANJIN UNIV