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Doped-state spherical FeF<3>.0.33H<2>O positive electrode material and preparation method therefor

A positive electrode material, spherical technology, applied in the field of new energy material preparation, can solve the problems of poor electrochemical performance, low electronic conductivity of ferric fluoride, low tap density, etc., to achieve high tap density, excellent electrochemical performance, rough surface effect

Inactive Publication Date: 2016-08-10
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The object of the present invention is to provide a doped spherical FeF 3 0.33H 2 O cathode material and preparation method thereof

Method used

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  • Doped-state spherical FeF&lt;3&gt;.0.33H&lt;2&gt;O positive electrode material and preparation method therefor
  • Doped-state spherical FeF&lt;3&gt;.0.33H&lt;2&gt;O positive electrode material and preparation method therefor
  • Doped-state spherical FeF&lt;3&gt;.0.33H&lt;2&gt;O positive electrode material and preparation method therefor

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Embodiment 1

[0034] At room temperature, weigh 4.04g Fe(NO 3 ) 3 9H 2 O, 0.384g Mg(NO 3 ) 2 ·6H 2 O was placed in a polytetrafluoroethylene reactor, and 50 mL of anhydrous methanol was added, magnetically stirred to dissolve, and 2 mL of HF aqueous solution with a mass fraction of 40% was added dropwise under constant stirring, and stirred for 15 minutes. Put the reactor in a hydrothermal reaction kettle and seal it, and heat it at 180°C for 6 hours to obtain a mixed solution with a layer of sediment on the bottom and a clarified upper part. Pour off the supernatant, wash the precipitate into a centrifuge tube with absolute ethanol and centrifuge to obtain a white Precipitate, wash twice with ethanol, centrifuge, and vacuum dry at 80°C for 12 hours to obtain white Fe 0.87 Mg 0.13 f 2.87 0.33H 2 O powder, by testing it was found that the Fe 0.87 Mg 0.13 f 2.87 0.33H 2 O is a spherical particle with a particle size of about 500 nm.

Embodiment 2

[0036] At room temperature, weigh 4.04g Fe(NO 3 ) 3 9H 2 O, 0.256g Mg(NO 3 ) 2 ·6H 2 O was placed in a polytetrafluoroethylene reactor, and 50 mL of anhydrous methanol was added, stirred magnetically to dissolve, and 2 mL of HF aqueous solution with a mass fraction of 40% was added dropwise under continuous stirring, and stirred for 10 minutes. Put the reactor in a hydrothermal reaction kettle and seal it, and heat it at 180°C for 6 hours to obtain a mixed solution with a layer of sediment on the bottom and a clarified upper part. Pour off the supernatant, wash the precipitate into a centrifuge tube with absolute ethanol and centrifuge to obtain a white Precipitate, wash twice with ethanol, centrifuge, and vacuum dry at 60°C for 16 hours to obtain white Fe 0.91 Mg 0.09 f 2.91 0.33H 2 O powder, by testing it was found that the Fe 0.91 Mg 0.09 f 2.91 0.33H 2 O is a spherical particle with a particle size of about 1 micron.

Embodiment 3

[0038] At room temperature, weigh 4.04g Fe(NO 3 ) 3 9H 2 O, 0.512g Mg(NO 3 ) 2 ·6H 2 O was placed in a polytetrafluoroethylene reactor, and 50 mL of anhydrous methanol was added, stirred magnetically to dissolve, and 2.1 mL of HF aqueous solution with a mass fraction of 45% was added dropwise under constant stirring, and stirred for 15 minutes. Put the reactor in a hydrothermal reaction kettle and seal it, and heat it at 190°C for 6 hours to obtain a mixed liquid covered with a layer of precipitate on the bottom and clear on the upper part. Pour off the supernatant, wash the precipitate into a centrifuge tube with absolute ethanol and centrifuge to obtain a white Precipitated, washed with ethanol for 3 times, centrifuged, and vacuum dried at 80°C for 12 hours to obtain white Fe 0.83 Mg 0.17 f 2.83 0.33H 2 O powder, by testing it was found that the Fe 0.83 Mg 0.17 f 2.83 0.33H 2 O is a spherical particle with a particle size of about 600 nanometers.

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Abstract

The invention discloses a doped-state spherical FeF<3>.0.33H<2>O positive electrode material and a preparation method therefor. The chemical expression of the positive electrode material is Fe<1-x>M<x>F<3+(n-3)x>.0.33H<2>O, wherein M is doped elements Mg, Co, Ni or Zn; x is equal to 0.03-0.3; and n is the valance of the corresponding doped elements. The preparation method comprises the steps of putting Fe(NO<3>)<3>.9H<2>O into a reactor, adding nitrate of other doped metal; then adding alcohol, magnetically stirring for 10-20min to obtain a settled solution; then adding an HF water solution in a dropwise manner and stirring for 10-20min; moving the mixture to a hydrothermal reaction kettle to react, then carrying out solid-liquid separation; and carrying out vacuum drying at a temperature of 20-80 DEG C to obtain the doped-state spherical FeF<3>.0.33H<2>O particles. The doped state spherical ferric fluoride obtained by the invention has uniform particles, rough surface, high tap density, high repeatability and excellent electrochemical performance; and the reaction yield can reach greater than 80%.

Description

technical field [0001] The invention relates to a doped state spherical FeF 3 0.33H 2 O cathode material and preparation method thereof, FeF 3 0.33H 2 O-doped spherical FeF 3 0.33H 2 The O material can be used as a positive electrode material of a lithium-ion battery, and belongs to the technical field of new energy material preparation. Background technique [0002] The research on lithium-ion battery electrode materials is currently a hot spot in the field of materials research, because energy storage equipment is the bottleneck restricting the development of the information age, and the modern society with high consumption cannot continue without continuous and efficient energy support. Through decades of continuous exploration by researchers all over the world, people have become very familiar with lithium-ion batteries, and have developed many commercial electrode materials, including positive electrode materials: lithium cobaltate, lithium manganate, ternary mater...

Claims

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Application Information

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IPC IPC(8): H01M4/58H01M10/0525C01G49/00
CPCC01G49/009C01P2004/03C01P2004/04C01P2004/62H01M4/58H01M10/0525H01M2004/021Y02E60/10
Inventor 刘黎郭国雄王先友陈晓莹易玲光舒洪波杨秀康
Owner XIANGTAN UNIV
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