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Preparation method of positive material sodium hexafluoroferrate applicable for sodium or lithium ion batteries and clad material thereof

A technology of sodium hexafluoroferrate and lithium ion battery, applied in battery electrodes, secondary batteries, circuits, etc., can solve the problem of low electrical conductivity of sodium hexafluoroferrate material, impurities in sodium hexafluoroferrate material, and cycle performance. To achieve the effect of uniform and controllable particle size, good fluidity and good crystallization performance

Inactive Publication Date: 2017-10-24
HUNAN INSTITUTE OF ENGINEERING
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  • Description
  • Claims
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Problems solved by technology

[0003] In 2012, Kisuk Kang of Seoul National University and Jang Wook Choi of Korea Advanced Institute of Science and Technology proposed carbon-coated sodium hexafluoroferrate (Na 3 FeF 6 ) as lithium-ion battery and sodium-ion battery cathode material, NaF and FeF 3 After high-energy ball milling in an argon atmosphere, and then coated with carbon as the positive electrode of the battery, it was found that Na in the sodium-ion battery 3 FeF 6 The discharge specific capacity is 111mAh / g (0.5 ~ 4.25V), the Na in the lithium ion battery 3 FeF 6 The discharge specific capacity is 241mAh / g (0.5 ~ 4.25V), the cycle performance of both is poor, and the capacity retention rate after 20 cycles is only about 50%.
They analyzed that the carbon-coated sodium hexafluoroferrate material prepared by the high-energy ball milling method contains impurities, coarse particles, uneven particle size, serious agglomeration, and the low conductivity of the sodium hexafluoroferrate material itself is the main cause of its poor cycle performance. reason

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  • Preparation method of positive material sodium hexafluoroferrate applicable for sodium or lithium ion batteries and clad material thereof
  • Preparation method of positive material sodium hexafluoroferrate applicable for sodium or lithium ion batteries and clad material thereof
  • Preparation method of positive material sodium hexafluoroferrate applicable for sodium or lithium ion batteries and clad material thereof

Examples

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Embodiment 1

[0035] Example 1: Weigh about 100 g of sodium sulfate, ferric sulfate and ammonium fluoride at a molar ratio of Na:Fe:F=3:1:6, dissolve them in deionized water at 10°C, and prepare sodium sulfate solution, sulfuric acid Iron solution and ammonium fluoride solution, the first two solutions are mixed to obtain a mixed solution of sodium sulfate and ferric sulfate. Under the action of mechanical stirring at a speed of 200rpm, ammonium fluoride solution was added to the mixed solution. After reacting for 3 hours, stop stirring, let stand for 5 hours, filter, wash with deionized water for 3 times, and vacuum dry at 120°C for 4 hours to obtain Sodium hexafluoroferrate material.

[0036] Put carbon black and sodium hexafluoroferrate into the ball milling tank at a mass ratio of 10:90, and add absolute ethanol. After ball milling at a speed of 400rpm for 5h, dry the product at 60°C in an air atmosphere for 10h, and crush Grading to obtain the carbon black-coated sodium hexafluoroferr...

Embodiment 2

[0037] Example 2: Weigh about 100 g of sodium nitrate, ferric nitrate and hydrofluoric acid at a molar ratio of Na:Fe:F=3:1:6, dissolve them in deionized water at 25° C., and prepare sodium nitrate solution, nitric acid Iron solution and ammonium fluoride solution, the first two solutions are mixed to obtain a mixed solution of sodium nitrate and ferric nitrate. Under the action of mechanical stirring at a speed of 300rpm, add the mixed solution and the ammonium fluoride solution into the reactor at the same time, after reacting for 4 hours, stop stirring, let stand for 8 hours, filter, wash with deionized water 4 times, and dry in vacuum at 100°C 6h, namely sodium hexafluoroferrate material.

[0038]Put carbon nanotubes and sodium hexafluoroferrate into a ball milling tank at a mass ratio of 5:95, and add absolute ethanol. After ball milling at a speed of 500 rpm for 4 hours, dry the product at 60°C in an air atmosphere for 12 hours. After crushing and classifying, the carbo...

Embodiment 3

[0039] Example 3: Weigh about 100 g of sodium fluoride, ferric chloride and ammonium fluoride at a molar ratio of Na:Fe:F=3:1:6, dissolve them in deionized water at 40°C, and prepare sodium fluoride solution, ferric chloride solution and ammonium fluoride solution, the latter two solutions are mixed to obtain a mixed solution of ferric chloride and ammonium fluoride. Under the action of mechanical stirring at a speed of 400rpm, add the mixed solution and sodium fluoride solution into the reactor at the same time. After reacting for 5 hours, stop stirring, let it stand for 10 hours, filter, wash with deionized water for 5 times, and vacuum dry at 90°C. After 10 hours, the sodium hexafluoroferrate material was obtained.

[0040] Add graphene and sodium hexafluoroferrate materials into the ball mill tank at a mass ratio of 2:98, and add acetone. After ball milling at a speed of 600rpm for 3 hours, the product is dried at 80°C for 8 hours in a nitrogen atmosphere, broken and class...

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Abstract

The invention discloses a preparation method of positive material sodium hexafluoroferrate applicable for sodium or lithium ion batteries and a clad material thereof. Sodium hexafluoroferrate sediment is prepared in a water solution by controlling the conditions of synthetic process, the sodium hexafluoroferrate material can be obtained through filtering and drying, and then the sodium hexafluoroferrate is mixed with a clad layer substance or a precursor thereof, so that the sodium hexafluoroferrate clad material is prepared through calcinations under different atmospheres. The sodium hexafluoroferrate material obtained in the invention is good in crystallization property and free of impurity phase; the particle morphology is regular, the particle size is uniform and controllable, and the mobility is good; and the sodium hexafluoroferrate and the clad material thereof are high in specific capacity and high in cycle stability. The preparation method is simple in technology, low in energy consumption, little in pollution and good in product performance, and is extremely applicable for industrial production.

Description

technical field [0001] The invention relates to the technical field of new materials, in particular to a preparation method of sodium hexafluoroferrate, a positive electrode material suitable for sodium or lithium ion batteries, and a coating material thereof. Background technique [0002] Sodium-ion batteries are not a new chemical power system. In the 1970s and 1980s, sodium-ion batteries and lithium-ion batteries were simultaneously researched. Since Japan's Sony Corporation commercialized lithium-ion batteries in the early 1990s, research on sodium-ion batteries slowed down for a time. With the advent of the era of electric vehicles and smart grids, the development of lithium-ion batteries is restricted by the bottleneck of lithium resource shortage. Compared with lithium, sodium reserves are very abundant, widely distributed and easy to extract. The physical and chemical properties of sodium and lithium are similar, and the charging and discharging principles of batt...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M4/62H01M10/0525H01M10/054
CPCH01M4/366H01M4/582H01M4/62H01M4/625H01M10/0525H01M10/054Y02E60/10
Inventor 刘万民唐俊秦牡兰邓继勇
Owner HUNAN INSTITUTE OF ENGINEERING
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