Preparation method and application of graphene-wrapping fluorine-doped lithium titanate nanowire

A graphene-coated, lithium fluorotitanate technology, applied in nanotechnology, nanotechnology, nanotechnology for materials and surface science, etc., can solve uneven mixing, uneven fluorine doping, difficult doping amount Determine and other issues to achieve the effect of low cost, uniform doping, and improved conductivity

Active Publication Date: 2018-07-17
CENT SOUTH UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The research on fluorine-doped lithium titanate and graphene-coated lithium titanate has been reported, but most of them are obtained by directly mixing lithium fluoride with titanium source and lithium source in sintering treatment by solid-phase method, as disclosed in patent number CN103346308A reported method, but the direct solid phase method for fluorine doping will cause uneven fluorine doping due to uneven mixing and the difficulty in determining the doping amount.

Method used

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  • Preparation method and application of graphene-wrapping fluorine-doped lithium titanate nanowire
  • Preparation method and application of graphene-wrapping fluorine-doped lithium titanate nanowire
  • Preparation method and application of graphene-wrapping fluorine-doped lithium titanate nanowire

Examples

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Embodiment 1

[0058] Weigh 24g NaOH and dissolve in 60mL deionized water, and weigh 0.6g industrialized TiO 2 Pour it into it and add 3mL of graphene oxide, stir at room temperature for 2h on a magnetic stirrer, then ultrasonicate for 2h, pour the mixture into a 100mL hydrothermal reactor and react in an oven at 200°C for 24h, then take out the reactant and wash it with deionized water several times, filtered and aged in dilute hydrochloric acid solution with pH 3 for 3h to obtain H 2 Ti 3 o 7 Nanowires.

[0059] Mix the obtained titanate nanowires with 50 mL of LiOH solution (0.5 mol / L), and add 0.05 g of NH 4 After F, pour them into an 80mL reactor, react at 150°C for 24h, take out, wash, filter and dry, and then sinter in an argon atmosphere furnace at 450°C for 3h to obtain graphene-coated fluorine-doped Li 4 Ti 5 o 12 Nanowires.

[0060] figure 1 It is the TEM picture made in Example 1. It can be seen from the figure that the lithium titanate nanowire material synthesized by th...

Embodiment 2

[0064] Weigh 24g NaOH and dissolve it in 60mL deionized water, weigh 1g industrialized TiO2 and pour it into it, add 3mL graphene oxide, stir at room temperature on a magnetic stirrer for 2h, then ultrasonicate for 2h, pour the mixture into a 100mL hydrothermal reaction kettle React in an oven at 180°C for 36 hours, then take out the reactant and wash it several times with deionized water, filter and age in a dilute hydrochloric acid solution with a pH of 3 for 3 hours to obtain H 2 Ti 3 o 7 Nanowires.

[0065] Mix the obtained titanate nanowires with 50 mL of LiOH solution (0.5 mol / L), and add 0.03 g of NH 4 After F, pour them into an 80mL reactor, react at 200°C for 36h, take out, wash, filter and dry, and then sinter in an argon atmosphere furnace at 450°C for 3h to obtain graphene-coated fluorine-doped Li 4 Ti 5 o 12 Nanowires.

[0066] image 3 This is the SEM image of the graphene-coated lithium fluorotitanate nanowires synthesized in Example 2. It can be seen fro...

Embodiment 3

[0069] Weigh 30g NaOH and dissolve in 60mL deionized water, and weigh 0.6g industrialized TiO 2 Pour it into it and add 3mL of graphene oxide, stir at room temperature for 2h on a magnetic stirrer, then ultrasonicate for 2h, pour the mixture into a 100mL hydrothermal reaction kettle and react in an oven at 150°C for 48h, then take out the reactant and wash it with deionized water several times, filtered and aged in dilute hydrochloric acid solution with pH 3 for 4h to obtain H 2 Ti 3 o 7 Nanowires.

[0070] Mix the obtained titanate nanowires with 50mL of LiOH solution (0.5mol / L), add 0.035g of LiF and pour them into an 80mL reaction kettle together, react at 200°C for 36h, take out, wash, filter and dry, then place in argon Fluorine-doped Li 4 Ti 5 o 12 Nanowires.

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Abstract

The invention provides a preparation method and application of a graphene-wrapping fluorine-doped lithium titanate nanowire and belongs to the technical field of lithium-ion battery energy material production. According to the preparation method, industrial-grade TiO2 which is low in cost is used as a raw material, a hydrothermal method is used as a basis, through two-step conversion, industrial-grade TiO2 which is low in cost is converted into the lithium titanate nanowire in a specific shape, the cost of forming the lithium titanate nanowire is greatly lowered, and industrial production andapplication are facilitated. Meanwhile, the lithium titanate nanowire is doped with liquid-phase fluorine and wrapped by graphene in situ, and the electric conductivity of the lithium titanate material is increased through the synergistic effect of the shape, ion doping and graphene wrapping. The obtained graphene-in-situ-wrapping fluorine-doped lithium titanate nanowire has the charging and discharging specific capacity close to a theoretical value, and the rate capability of the material is remarkably increased.

Description

technical field [0001] The invention belongs to the technical field of lithium ion batteries, and in particular relates to a preparation method and application of graphene-coated fluorine-doped lithium titanate nanowires. Background technique [0002] With the intensification of the global energy crisis and environmental problems, especially the combustion of fossil fuels and the emission of vehicle exhaust have caused great harm to the environment, it is of great significance to develop clean and efficient energy. Under such a background, supercapacitors and lithium-ion batteries emerged as the times require, and are widely used in various fields such as electronics, transportation, and energy storage. [0003] Lithium titanate (Li 4 Ti 5 o 12 ) as an electrode material for a new type of energy storage battery is gaining more and more attention. This is due to the small change in lattice constant of spinel lithium titanate when lithium ions are intercalated and extracted...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/36H01M4/485H01M4/62H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/485H01M4/625H01M10/0525H01M2004/021H01M2004/027Y02E60/10
Inventor 胡国荣杜柯彭忠东曹雁冰吴吉林杨浩
Owner CENT SOUTH UNIV
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