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A carbon-coated sodium iron phosphate-sodium vanadium phosphate composite material and preparation method thereof

A technology of sodium iron phosphate and sodium vanadium phosphate, applied in electrical components, electrochemical generators, battery electrodes, etc., can solve the problems of high sintering temperature and poor cycle performance, and achieve low synthesis temperature, good cycle performance, high The effect of conductivity

Active Publication Date: 2017-11-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sintering temperature of the method is high, and when the prepared sodium vanadium phosphate composite material is used as a positive electrode, the initial discharge capacity is 92-109mAh·g -1 , and poor cycle performance at high rates

Method used

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  • A carbon-coated sodium iron phosphate-sodium vanadium phosphate composite material and preparation method thereof
  • A carbon-coated sodium iron phosphate-sodium vanadium phosphate composite material and preparation method thereof
  • A carbon-coated sodium iron phosphate-sodium vanadium phosphate composite material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Add 500mLNH 4 VO 3solution (2mol / L) and 500mL Fe(NO 3 ) 3 Solution (2mol / L, by Fe(NO 3 ) 3 9H 2 O) were added dropwise into the continuous reaction kettle at a rate of 5mL / min, stirred and reacted at 60°C with a stirring speed of 250r / min, and the pH value of the solution was continuously adjusted to 5.0 by 3mol / L ammonia water, dropwise After the addition, age at 50°C for 12 hours, filter, and wash the filter residue 3 times with distilled water to obtain hydrated ferric vanadate; (2) Place the hydrated ferric vanadate obtained in step (1) in a tube furnace, In an air atmosphere, sinter at 450°C for 5 hours to obtain iron vanadate; (3) mix 0.04mol (6.84g) of iron vanadate obtained in step (2) with 0.1mol (15.6g) of NaH 2 PO 4 2H 2 O, 0.085mol (7.65g) oxalic acid and 0.0012mol (0.216g) glucose were placed in a ball mill jar, and then 80mL of ethanol was added as a dispersant, mixed evenly, ball milled at a speed of 250r / min for 4h, and then placed in an oven...

Embodiment 2

[0040] (1) Add 500mLNH 4 VO 3 solution (1mol / L) and 500mL Fe(NO 3 ) 3 Solution (1mol / L, made of Fe(NO 3 ) 3 9H 2 O) were added dropwise into the continuous reaction kettle at a rate of 3mL / min, stirred and reacted at 40°C with a stirring speed of 200r / min, and the pH value of the solution was continuously adjusted to 3.0 by 1mol / L ammonia water, dropwise After the addition is completed, age at 30°C for 6 hours, filter, and wash the filter residue 3 times with distilled water to obtain hydrated ferric vanadate; (2) Place the hydrated ferric vanadate obtained in step (1) in a tube furnace, Under air atmosphere, sinter at 400°C for 2 hours to obtain iron vanadate; (3) mix 0.04mol (6.84g) of iron vanadate obtained in step (2) with 0.1mol (15.6g) of NaH 2 PO 4 2H 2 O, 0.028mol (2.52g) oxalic acid and 0.0008g (0.144g) glucose were placed in a ball mill jar, then 35mL of ethanol was added as a dispersant, mixed evenly, ball milled at a speed of 100r / min for 2h, and then place...

Embodiment 3

[0043] (1) Add 500mLNH 4 VO 3 solution (3mol / L) and 500mL Fe(NO 3 ) 3 Solution (3mol / L, by Fe(NO 3 ) 3 9H 2 O) were added dropwise into the continuous reaction kettle at a rate of 7mL / min, stirred and reacted at 75°C with a stirring speed of 300r / min, and the pH value of the solution was continuously adjusted to 6.0 by 5mol / L ammonia water, dropwise After the addition is completed, age at 70°C for 15 hours, filter, and wash the filter residue 3 times with distilled water to obtain ferric vanadate hydrate; (2) place the ferric vanadate hydrate obtained in step (1) in a tube furnace, Under air atmosphere, sinter at 500°C for 10 hours to obtain iron vanadate; (3) mix 0.04mol (6.84g) of iron vanadate obtained in step (2) with 0.1mol (15.6g) of NaH 2 PO 4 2H 2 O, 0.14mol (12.6g) oxalic acid and 0.0015mol (0.27g) glucose were placed in a ball mill jar, and then 100mL of ethanol was added as a dispersant, mixed evenly, ball milled at a speed of 300r / min for 6h, and then place...

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Abstract

The invention discloses a carbon-coated iron phosphate sodium-vanadium phosphate sodium composite material and a preparation method thereof. The preparation method comprises the steps that 1, an NH4VO3 solution and a Fe(NO3)3 solution are dropwise added into a continuous reaction kettle for stirring and reaction, after dropwise adding is finished, ageing, filtering and filter residue washing are carried out, and hydration ferric vanadate is obtained; 2, sintering is carried out in air atmosphere, and ferric vanadate is obtained; 3, the ferric vanadate, NaH2PO4.2H2O, glucose and oxalic acid are placed in a ball milling tank, then ethyl alcohol is added, and ball milling and drying are carried out; 4, milling returning is carried out; 5, calcination is carried out in inert atmosphere, and the carbon-coated iron phosphate sodium-vanadium phosphate sodium composite material is obtained. The carbon-coated iron phosphate sodium-vanadium phosphate sodium composite material is excellent in electrochemical performance, can be used as a positive electrode material of a secondary sodium ion battery, has the high gram volume, is high in safety and can be applied to energy storage devices, back-up power sources, reserved power sources and the like. The preparation method is low in resultant temperature and simple in technology.

Description

technical field [0001] The invention relates to a sodium ion battery cathode material and a preparation method thereof, in particular to a carbon-coated sodium iron phosphate-sodium vanadium phosphate composite material and a preparation method thereof. Background technique [0002] Lithium iron phosphate-lithium vanadium phosphate composite material is the product of modifying lithium iron phosphate by using the advantages of high ion conductivity, high theoretical specific capacity and high discharge platform of lithium vanadium phosphate. After modification, it has high theoretical specific capacity, Good thermal stability and other advantages. CN 104485448 A discloses a method for solvothermally synthesizing lithium iron phosphate-lithium vanadium phosphate composite material in one step, and synthesizes a lithium iron phosphate-lithium vanadium phosphate composite material with better low-temperature performance, but this method has a large amount of wastewater and is d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/58H01M4/583H01M4/62H01M10/054
CPCH01M4/362H01M4/366H01M4/5825H01M4/583H01M4/625H01M10/054Y02E60/10
Inventor 张佳峰刘益张宝明磊王小玮田业成
Owner CENT SOUTH UNIV