Method for preparing sodium fluorophosphate vanadium for positive pole material of sodium-ion battery

A technology of sodium vanadium fluorophosphate and sodium ion battery, which is applied to battery electrodes, circuits, electrical components, etc., can solve the problems of poor charge and discharge performance, long synthesis cycle, coarse product particles, etc., and achieves low synthesis temperature and short synthesis cycle. , the effect of a simple synthesis method

Inactive Publication Date: 2013-04-03
广西地博矿业集团股份有限公司
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

The traditional preparation methods mainly include high-temperature solid-phase sintering method, carbothermal reduction method, sol-gel method, etc. These methods all require the preparation of sodium vanadium fluorophosphate by carbothermal reduction of vanadium under high temperature conditions, so the synthesis temperature is high and the synthesis period is high. Long and the obtained product particles are relatively coarse, and the charge and discharge performance is poor

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  • Method for preparing sodium fluorophosphate vanadium for positive pole material of sodium-ion battery
  • Method for preparing sodium fluorophosphate vanadium for positive pole material of sodium-ion battery

Examples

Experimental program
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Effect test

Embodiment 1

[0015] Using vanadium pentoxide, ammonium dihydrogen phosphate, sodium carbonate, hydrofluoric acid and lactic acid as raw materials, mix evenly according to the molar ratio of vanadium: phosphorus: sodium: fluorine element 1:1:1:1; then press lactic acid : The molar ratio of vanadium pentoxide is 1:1, adding reducing agent to mechanical activation (ball milling) for 0.5 hours, under normal temperature and pressure conditions, the reducing agent will reduce high-valent vanadium to form fine particles of amorphous sodium vanadium fluorophosphate; will The amorphous sodium vanadium fluorophosphate in step is loaded into a tube furnace, heated to 500°C, 550°C, 650°C and 750°C in an argon atmosphere, and calcined at a constant temperature for 2 hours to obtain crystalline powder. It was analyzed by X-ray diffraction as sodium vanadium fluorophosphate (NaVPO 4 F) Structure.

[0016] The resulting vanadium vanadium phosphate product was assembled into a button battery to measure ...

Embodiment 2

[0020] Using vanadium dioxide, triammonium phosphate, sodium fluoride and malic acid as raw materials, mix evenly according to the molar ratio of vanadium: phosphorus: sodium: fluorine element 1:1:1:1; The molar ratio of vanadium is 5:1, adding reducing agent to mechanical activation (ball milling) for 24 hours, under the condition of normal temperature and pressure, the reducing agent will reduce the high-valent vanadium to produce fine particles of amorphous sodium vanadium fluorophosphate;

[0021] Put the amorphous sodium vanadium fluorophosphate in step into a tube furnace, heat to 700°C in a hydrogen atmosphere, and calcine at a constant temperature for 0.5 hours, 5 hours, 8 hours and 24 hours respectively to obtain a crystalline state powder. It was analyzed by X-ray diffraction as sodium vanadium fluorophosphate (NaVPO 4 F) Structure.

[0022] The obtained sodium vanadium fluorophosphate product was assembled into a button battery to measure its charge-discharge sp...

Embodiment 3

[0026] Using ammonium metavanadate, diammonium hydrogen phosphate, sodium fluoride and acetaldehyde as raw materials, mix evenly according to the molar ratio of vanadium: phosphorus: sodium: fluorine element 1:1:1:1; then use acetaldehyde: The molar ratio of ammonium metavanadate is 10:1, adding a reducing agent for mechanical activation (ball milling) for 8 hours. Under normal temperature and pressure conditions, the reducing agent reduces the high-valent vanadium to form fine particles of amorphous sodium vanadium fluorophosphate;

[0027] Put the amorphous sodium vanadium fluorophosphate in the step into a tube furnace, heat to 560°C in a nitrogen atmosphere, and calcine at a constant temperature for 15 hours to obtain crystalline powder. It was analyzed by X-ray diffraction as sodium vanadium fluorophosphate (NaVPO 4 F) Structure.

[0028] Assemble the obtained sodium vanadium fluorophosphate product into a button battery to measure its charge-discharge specific capacit...

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Abstract

The invention discloses a method for preparing sodium fluorophosphate vanadium for a positive pole material of a sodium-ion battery. The method comprises the following steps of: taking a high-valence vanadium source compound, a phosphorus source compound, a sodium source compound, a fluorine source compound and a reductant as raw materials, and uniformly mixing the raw materials in a manner that the molar ratio of vanadium to phosphorus to sodium to fluorine is 1: 1: (1-1.05): 1; adding the reductant in a manner that the molar ratio of the reductant to the vanadium source compound is (1: 1) to (10: 1), carrying out mechanical activation for 0.5-24 hours, and producing small-particle amorphous sodium fluorophosphate vanadium under the conditions of normal temperature and normal pressure in a manner that high-valence vanadium is reduced by the reductant; and heating the amorphous sodium fluorophosphate vanadium to the temperature of 500-750 DEG C in a non-oxidizing atmosphere, and carrying out constant-temperature calcination for 0.5-24 hours, thereby obtaining crystalline-state sodium fluorophosphate vanadium powder. The method has the advantages that the synthesis temperature is low, the synthesis cycle is short, the synthesis method is simple, the quality of synthetic products is high, and the large-scale industrialized preparation of the sodium fluorophosphate vanadium for the positive pole material of the sodium-ion battery is easily realized.

Description

technical field [0001] The invention belongs to the technical field of electrode materials, and in particular relates to a preparation method of sodium vanadium fluorophosphate, a positive electrode material of a sodium ion battery. Background technique [0002] Sodium vanadium fluorophosphate (NaVPO 4 F) is a new type of anode material for sodium-ion batteries. It has a stable structure, a charge-discharge platform up to 3.7V, and good cycle performance. It is a very promising anode material for sodium-ion batteries. The traditional preparation methods mainly include high-temperature solid-phase sintering method, carbothermal reduction method, sol-gel method, etc. These methods all require the preparation of sodium vanadium fluorophosphate by carbothermal reduction of vanadium under high temperature conditions, so the synthesis temperature is high and the synthesis period is high. Long and the obtained product particles are relatively coarse, and the charge and discharge p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/58
CPCY02E60/10
Inventor 寇文胜陈国民李秀兰陈晓明李晓青孙文忠池上荣周若水李玉保蒙有言都安治刘恩义
Owner 广西地博矿业集团股份有限公司
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