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Preparation and application of ferric fluoride doping nano titanium dioxide

A technology of nano-titanium dioxide and ferric fluoride, which is applied in secondary batteries, electrochemical generators, electrical components, etc., can solve the problems of difficulty in preparation, rising cost, and high-temperature hydrolysis, and achieve excellent cycle performance and actual capacity , The effect of simple preparation method

Active Publication Date: 2019-03-19
CHINA UNIV OF MINING & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of preparation and storage of fluoride, it is easy to form crystalline hydrate, and the dehydration process is prone to high-temperature hydrolysis, which greatly increases the difficulty and cost of preparation.
Currently no FeF 3 (H 2 O) X / TiO 2 Literature reports on composite materials

Method used

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  • Preparation and application of ferric fluoride doping nano titanium dioxide
  • Preparation and application of ferric fluoride doping nano titanium dioxide
  • Preparation and application of ferric fluoride doping nano titanium dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] First weigh 0.1gTiO 2 Dissolve completely in 30ml of distilled water as a milky white liquid, then let it stand for 12-16 hours, then add 4mg of cetyltrimethylammonium bromide and 20.2g of Fe(NO 3 ) 3 .9H 2 O was stirred with a glass rod in an ultrasonic wave to dissolve it completely, and it appeared as a brownish-yellow liquid; after stirring for 10 minutes, place it in a polytetrafluoroethylene plastic bottle, add 12ml of 40% hydrofluoric acid to become colorless, and stir for 24 hours Turn into a pink liquid; then add isopropanol dropwise until the solution turns into a colorless liquid, stir for 30 minutes, then heat up to 80°C, heat and stir for 24 hours to evaporate excess hydrofluoric acid and water, and obtain light yellow FeF 3 (H 2 0) 4.5 / TiO 2 ; then vacuum-dried at 80°C for 24h in a vacuum oven, and then vacuum-dried at 120°C for 24h in a vacuum oven to obtain light green FeF 3 (H 2 0) X / TiO 2 .

[0027] figure 1 It is the XRD spectrum of synth...

Embodiment 2

[0040] First weigh 0.05gTiO 2 It was completely dissolved in 15ml of distilled water, and it was a milky white liquid. Then it was allowed to stand for 6 hours, and then 2mg of dodecyltrimethylammonium bromide and 10.1g of Fe(NO 3 ) 3 .9H 2 O was stirred with a glass rod in an ultrasonic wave to dissolve it completely, and it appeared as a brownish-yellow liquid; after stirring for 20 minutes, it was placed in a polytetrafluoroethylene plastic bottle, and 5.43ml of hydrofluoric acid with a mass fraction of 40% was added to become colorless, and stirred After 12 hours, it turns into a pink liquid; add isopropanol dropwise until the solution turns into a colorless liquid, stir for 30 minutes, then heat up to 90°C, heat and stir for 18 hours to evaporate excess hydrofluoric acid and water, and obtain light yellow FeF 3 (H 2 0) 4.5 / TiO 2 ; then vacuum-dried in a vacuum oven at 90°C for 18h, and then vacuum-dried in a vacuum oven at 110°C for 18h to obtain light green FeF 3 ...

Embodiment 3

[0042] First weigh 0.1gTiO 2 Completely dissolved in 30ml of distilled water, it was a milky white liquid, then let it stand for 10h, then added 4mg of octadecyltrimethylammonium chloride and 20.2g of Fe(NO 3 ) 3 .9H 2 O was stirred with a glass rod in an ultrasonic wave to dissolve it completely, showing a brownish yellow liquid; after stirring for 30 minutes, place it in a polytetrafluoroethylene plastic bottle, add 26.09ml of hydrofluoric acid with a mass fraction of 20% to become colorless, stir After 18 hours, it turns into a pink liquid; add isopropanol dropwise until the solution turns into a colorless liquid, stir for 30 minutes, then heat up to 100°C, heat and stir for 12 hours to evaporate excess hydrofluoric acid and water, and obtain light yellow FeF 3 (H 2 0) 4.5 / TiO 2 ; then vacuum-dried in a vacuum oven at 100°C for 12h, and then vacuum-dried in a vacuum oven at 130°C for 12h to obtain light green FeF 3 (H 2 0) X / TiO 2 .

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Abstract

The invention discloses a preparation and application of ferric fluoride doping nano titanium dioxide. The ferric fluoride doping nano titanium dioxide is prepared by adopting ferric nitrate, hydrofluoric acid and TiO2 as raw materials in a liquid phase method. The preparation method comprises the following steps: (1) measuring TiO2 powder, incompletely dispersing in distilled water, standing for6 to 12 hours, adding surfactant and Fe(NO3)3.9H2O, and ultrasonically stirring and completely dissolving to obtain brownish liquid; (2) stirring for 10 to 30 min, placing in a polytetrafluoroethyleneplastic bottle, adding hydrofluoric acid, and stirring for 12 to 24 hours to obtain pink liquid; (3) adding isopropanol or absolute ethyl alcohol until the solution is colorless, stirring for 30 to 40 min, heating to 80 to 100 DEG C, heating and stirring for 12 to 24 hours, and evaporating to remove surplus hydrofluoric acid and water to obtain flavescent FeF3(H2O)4.5 / TiO2; and (4) vacuum dryingfor 12 to 24 hours at 110 to 130 DEG C to obtain laurel-green FeF3(H2O)X / TiO2. The preparation method of the invention is simple, short in process and good in repetition; the first discharge capacityof FeF3(H2O)X / TiOx is 512mAh / g and is approximate to a theoretical value, and the ferric fluoride doping nano titanium dioxide has excellent cycling performance and actual capacity and can be used asa lithium ion battery anode material.

Description

technical field [0001] The invention belongs to the field of inorganic functional materials and relates to a nanocomposite material, in particular to the preparation and application of ferric fluoride doped nano titanium dioxide. Background technique [0002] In recent years, the rapid development of electric tools, electric bicycles, especially electric vehicles and other fields has provided good application prospects for lithium-ion batteries, but at the same time, the cycle life, energy density, safety, price and environmental protection of lithium-ion batteries have been greatly affected. Capacitance and other performance put forward higher requirements. [0003] At present, some breakthroughs have been made in the research of binary iron fluoride (mainly iron trifluoride) as the positive electrode of lithium-ion batteries. It can achieve 2-3 times the capacity performance of traditional lithium intercalation electrode materials through reversible conversion reactions. ...

Claims

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Application Information

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IPC IPC(8): H01M4/36H01M4/48H01M4/58H01M10/0525
CPCH01M4/364H01M4/48H01M4/582H01M10/0525Y02E60/10
Inventor 史月丽刘雯庄全超崔永莉鞠治成
Owner CHINA UNIV OF MINING & TECH
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