Preparation method of sodium vanadium fluorophosphate positive electrode material

A technology of sodium vanadium fluorophosphate and positive electrode materials, which is applied in the field of positive electrode materials for sodium ion batteries, can solve the problems of unfavorable large-scale production, long reaction process, and high raw material prices, and achieve short preparation cycle, short transmission path, and good conductivity Effect

Inactive Publication Date: 2020-08-14
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to current reports, Na 3 V 2( PO 4 ) 2 f 3 The synthesis methods mainly include ball milling method, high-temperature solid-phase method, and hydrothermal method. These methods all have high temperature (600°C-700°C) and long-term (4h-12h) sintering process, so the preparation time is long and the energy consumption is high.
[0004] Chinese patent CN103594716A discloses a method for preparing sodium vanadium fluorophosphate positive electrode material through sol-gel activation-assisted two-step high-temperature solid-phase method. The material prepared by this method has the characteristics of good stability and uniform particle size, but the reaction process is long. high production cost
[0005] Chinese patent CN108682855A discloses a method for the controllable preparation of sodium vanadium fluorophosphate positive electrode material by hydrothermal method. The hydrothermal time is as long as 6 to 12 hours, the reaction process is very long, and the price of raw materials is high, which is not conducive to large-scale production.

Method used

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  • Preparation method of sodium vanadium fluorophosphate positive electrode material
  • Preparation method of sodium vanadium fluorophosphate positive electrode material
  • Preparation method of sodium vanadium fluorophosphate positive electrode material

Examples

Experimental program
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Effect test

Embodiment 1

[0028] a kind of Na 3 V 2 (PO 4 ) 2 f 3 The preparation method of C sodium ion cathode material comprises the following steps:

[0029] Step 1: Weigh ammonium metavanadate, ammonium dihydrogen phosphate and sodium fluoride according to the molar ratio of sodium, vanadium, phosphorus and fluorine elements of 3:2:2:3, dissolve them in deionized water, and then reduce them according to the vanadium Add oxalic acid to 1.5 times the theoretical molar amount required to form trivalent vanadium, and stir at 40°C for 15 minutes to obtain a dark green solution.

[0030] Step 2: Carry the solution prepared in step 1 into the spray pyrolysis reactor at a flow rate of 3L / min through the carrier liquid argon, and pyrolyze it at 750°C to obtain Na 3 V 2 (PO 4 ) 2 f 3 Microspheres.

[0031] Step 3: The resulting Na prepared in step 23 V 2 (PO 4 ) 2 f 3 The microspheres and acetylene black were added to the ball mill tank at a mass ratio of 9:1, and placed in a horizontal planet...

Embodiment 2

[0034] a kind of Na 3 V 2 (PO 4 ) 2 f 3 The preparation method of C sodium ion cathode material comprises the following steps:

[0035] Step 1: Weigh vanadium pentoxide, ammonium dihydrogen phosphate, sodium carbonate and ammonium fluoride according to the molar ratio of sodium, vanadium, phosphorus and fluorine elements of 3:2:2:3, dissolve them in deionized water, and then, according to Add oxalic acid to 1.5 times the theoretical molar amount required for vanadium to be reduced to trivalent vanadium, and stir at 60°C for 30 minutes to obtain a dark green solution.

[0036] Step 2: The solution prepared in step 1 is carried into the spray pyrolysis reactor by the carrier liquid argon at a flow rate of 3L / min, and sprayed and pyrolyzed at 750°C to obtain Na 3 V 2 (PO 4 ) 2 f 3 Microspheres.

[0037] Step 3: the Na prepared in step 2 3 V 2 (PO 4 ) 2 f 3 The microspheres and acetylene black were added to the ball mill tank at a mass ratio of 9:1, placed in a hori...

Embodiment 3

[0040] a kind of Na 3 V 2 (PO 4 ) 2 f 3 The preparation method of C sodium ion cathode material comprises the following steps:

[0041] Step 1: Weigh ammonium metavanadate, ammonium dihydrogen phosphate and sodium fluoride and dissolve them in deionized water according to the molar ratio of sodium, vanadium, phosphorus and fluorine elements of 3:2:2:3, and then, according to the vanadium is reduced to Add citric acid to 1.5 times the theoretical molar amount required for trivalent vanadium, and stir for 0.5 h at 60°C to obtain a dark green solution.

[0042] Step 2: Carry the solution prepared in step 1 into the spray pyrolysis reactor at a flow rate of 4 L / min through the carrier liquid argon, and the solution is sprayed and pyrolyzed at 700 ° C to obtain Na 3 V 2 (PO 4 ) 2 f 3 Microspheres.

[0043] Step 3: the Na prepared in step 2 3 V 2 (PO 4 ) 2 f 3 The microspheres and acetylene black were added to the ball mill tank at a mass ratio of 4:1, placed in a hor...

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Abstract

The invention provides a preparation method of a sodium vanadium fluorophosphate positive electrode material. The preparation method comprises the following steps: mixing a vanadium source, a phosphorus source, a sodium source, a fluorine source and an organic reducing agent to prepare a solution, carrying out spray pyrolysis to obtain Na3V2(PO4)2F3 microspheres, and carrying out mechanical ball milling on the Na3V2(PO4)2F3 microspheres and a carbon material to obtain a well-crystallized Na3V2(PO4)2F3/C material. Compared with the traditional ball milling method, the spray pyrolysis-mechanicalball milling method adopted by the invention has the advantages of high material synthesis speed, low energy consumption, high yield, simple process, easiness in operation and the like, and avoids the long-time sintering process of the raw materials at high temperature. The obtained Na3V2(PO4)2F3 microspheres and the final Na3V2(PO4)2F3/C material have spherical morphology and are relatively small in particle size. The prepared Na3V2(PO4)2F3/C material passes an electrochemical performance test, has relatively good specific discharge capacity, and has a relatively good application prospect ina sodium-ion battery positive electrode material.

Description

technical field [0001] The invention relates to the field of anode materials for sodium ion batteries, in particular to a preparation method for sodium vanadium fluorophosphate cathode materials. Background technique [0002] With the rapid development of the 3C field, new energy vehicles and new energy storage, lithium-ion batteries have been widely used. People are no longer satisfied with the energy density of existing devices, and the demand for lithium-ion batteries is also increasing. Since 2016, the price of lithium carbonate has continued to rise. It is worth noting that the abundance of lithium in the earth is about 0.0065%. Such a low amount of resources cannot bear the huge consumption of lithium resources. The development of lithium-ion batteries will undoubtedly be constrained by prices. Sodium-ion batteries are considered to be the best candidate power sources because sodium and lithium elements are in the same main group, adjacent in position, and have simil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58H01M4/62H01M10/054
CPCH01M4/5825H01M4/625H01M4/628H01M10/054H01M2004/028Y02E60/10
Inventor 颜果春胡蓉王接喜朱鹏飞李新海王志兴郭华军胡启阳彭文杰
Owner CENT SOUTH UNIV
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