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Preparation method of titanium-doping ferric fluoride positive electrode material

A cathode material, iron fluoride technology, which is applied in chemical instruments and methods, inorganic chemistry, battery electrodes, etc., can solve the problems of capacity decline and poor rate performance of iron fluoride cathode materials, and achieves a simple and easy synthesis process. The effect of low recession and high yield

Inactive Publication Date: 2017-02-22
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a method for preparing a titanium-doped iron fluoride cathode material for the problems of serious capacity fading and poor rate performance in the iron fluoride cathode material

Method used

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  • Preparation method of titanium-doping ferric fluoride positive electrode material
  • Preparation method of titanium-doping ferric fluoride positive electrode material
  • Preparation method of titanium-doping ferric fluoride positive electrode material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) First ferric chloride and titanium chloride are used as starting materials, according to Fe 3+ : Ti 3+ =0.92:0.08 molar ratio dissolved in ethanol, stirred evenly, to obtain a golden yellow transparent solution, wherein the iron ion concentration is 0.3mol / L;

[0038] (2) Slowly add the sodium hydroxide solution with a concentration of 1.5mol / L into the solution obtained in step (1), stir evenly, and age it statically for 36 hours to obtain a brown precipitate, which is repeatedly washed with ethanol and deionized water until the filtrate The pH value is 6-7, and air-dried at 80°C for 6 hours;

[0039] (3) Add 40mL of ionized water to the hydroxide precipitated powder obtained in step (2), and stir to obtain a suspension;

[0040] (4) Slowly add 20 mL of hydrogen fluoride solution to the suspension obtained in step (3), react in an oil bath at 30°C for 12 hours, and dissolve the suspension to obtain a pink solution;

[0041] (5) heat and stir the pink solution ob...

Embodiment 2

[0048] (1) First, ferric sulfate and titanium chloride are used as starting materials, according to Fe 3+ : Ti 3+ =0.50: Dissolve in ethanol at a molar ratio of 0.50 and stir evenly to obtain a golden yellow transparent solution, in which the concentration of iron ions is 0.25 mol / L.

[0049] (2) Slowly add the potassium hydroxide solution with a concentration of 1.25mol / L into the solution obtained in step (1), stir evenly, and age it statically for 36 hours to obtain a brown precipitate, which is repeatedly washed with ethanol and deionized water until the filtrate The pH value is 6-7, and air-dried at 80°C for 6 hours;

[0050] (3) Add 40mL of ionized water to the hydroxide precipitated powder obtained in step (2), and stir to obtain a suspension;

[0051] (4) Slowly add 20 mL of hydrogen fluoride solution to the suspension obtained in step (3), react in an oil bath at 30°C for 12 hours, and dissolve the suspension to obtain a pink solution;

[0052] (5) heat and stir th...

Embodiment 3

[0057] (1) First, ferric nitrate and titanium chloride are used as starting materials, according to Fe 3+ : Ti 3+ =0.91:0.09 molar ratio dissolved in ethanol, stirred evenly to obtain a golden yellow transparent solution, wherein the iron ion concentration is 0.4mol / L.

[0058] (2) Slowly add the sodium hydroxide solution with a concentration of 2.0mol / L into the solution obtained in step (1), stir evenly, and age it statically for 48 hours to obtain a brown precipitate, which is repeatedly washed with ethanol and deionized water until the filtrate The pH value is 6-7, and air-dried at 80°C for 6 hours;

[0059] (3) Add 40mL of ionized water to the hydroxide precipitated powder obtained in step (2), and stir to obtain a suspension;

[0060] (4) Slowly add 20 mL of hydrogen fluoride solution to the suspension obtained in step (3), react in an oil bath at 30°C for 12 hours, and dissolve the suspension to obtain a pink solution;

[0061] (5) heat and stir the pink solution obt...

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Abstract

The invention discloses a preparation method of a titanium-doping ferric fluoride positive electrode material. The general formula of the material is Fe<(1-x)>Ti<x>F<3>.0.33H<2>O / C, wherein x is more than or equal to 0.01 but less than or equal to 0.50. The material is obtained by the steps of dissolving a titanium salt and an iron salt, depositing a hydroxide, introducing fluorine ions to a hydrogen fluoride solution, performing deposition, dissolving and evaporation of the hydroxide to obtain a powder material, dehydrating the powder material, performing high-energy ball milling of a carbon material and performing processing. The Fe<(1-x)>Ti<x>F<3>.0.33H<2>O / C positive electrode material prepared according to the method has a complete orthorhombic crystal system, is relatively small in grain size, uniform in element distribution and good in charge / discharge performance, and has relatively high discharge specific capacity, excellent cycle performance and favorable rate performance, and the problem of poor cycle and rate performance of an existing FeF<3>.0.33H<2>O material is solved. The involved raw material is low in cost, the preparation process is simple, the preparation period is relatively short, and the preparation method has a good application prospect.

Description

technical field [0001] The invention relates to the field of lithium-ion battery cathode materials and electrochemistry, in particular to a preparation method of titanium-doped iron fluoride cathode materials. Background technique [0002] With the rapid increase in the number of batteries required in energy storage fields such as new energy vehicles, mobile communications, and wind power generation and grid support, lithium-ion batteries will usher in greater development opportunities. 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. From the perspective of the development of the entire positive and negative electrode materials, the key factor restricting the improvement of the energy density of lit...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/58H01M10/0525C01G49/00
CPCC01G49/009C01P2002/72C01P2004/03C01P2006/40H01M4/362H01M4/582H01M10/0525Y02E60/10
Inventor 王先友魏双英张蕊余睿智胡海申永强
Owner XIANGTAN UNIV
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