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A method for preparing nano-electrode material li4ti5o12/rutile-tio2 by composite solvothermal method

A nano-electrode, composite solvent technology, applied in nanotechnology, battery electrodes, nanotechnology and other directions, to achieve good solvent thermal critical reaction conditions, low viscosity, and reduce losses

Active Publication Date: 2021-10-22
LIAONING UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the solvothermal synthesis of Li 4 Ti 5 o 12 / Rutile-TiO 2 fewer reports

Method used

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  • A method for preparing nano-electrode material li4ti5o12/rutile-tio2 by composite solvothermal method
  • A method for preparing nano-electrode material li4ti5o12/rutile-tio2 by composite solvothermal method
  • A method for preparing nano-electrode material li4ti5o12/rutile-tio2 by composite solvothermal method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Dissolve 2.5mL of tetrabutyl titanate in 35mL of diethylene glycol and water mixed solution (2.5:1 by volume), and magnetically stir for 1 hour to make it evenly mixed to obtain a mixed solution;

[0037] (2) 0.268g LiOH·H 2 O was dissolved in 15mL of deionized water, and ultrasonically vibrated for half an hour to completely dissolve the lithium hydroxide to obtain an aqueous solution of lithium hydroxide;

[0038] (3) Add lithium hydroxide aqueous solution to the mixed solution obtained in step (1) drop by drop, after stirring for 5 hours, transfer the reaction solution to a 100mL stainless steel autoclave, and keep it at 180°C for 36 hours, and obtain a white precipitate after solvent heat treatment ; After being washed by centrifugation for 5 times and dried in an oven at 80°C, the precursor was obtained;

[0039] (4) Put the obtained precursor in a muffle furnace, calcinate in air atmosphere at 550-600°C for 6 hours, cool naturally to room temperature, and gri...

Embodiment 2

[0041] (1) Dissolve 2.5mL of tetrabutyl titanate in 35mL of diethylene glycol and water mixed solution (2.5:1 by volume), and magnetically stir for 1 hour to make it evenly mixed to obtain a mixed solution;

[0042] (2) 0.268g LiOH·H 2 O was dissolved in 15mL of deionized water, and ultrasonically vibrated for half an hour to completely dissolve the lithium hydroxide to obtain an aqueous solution of lithium hydroxide;

[0043] (3) Add lithium hydroxide aqueous solution to the mixed solution obtained in step (1) drop by drop, after stirring for 5 hours, transfer the reaction solution to a 100mL stainless steel autoclave, and keep it at 180°C for 36 hours, and obtain a white precipitate after solvent heat treatment ; After being washed by centrifugation for 5 times and dried in an oven at 80°C, the precursor was obtained;

[0044] (4) Place the obtained precursor in a muffle furnace, calcinate at 650-700°C for 6 hours in an air atmosphere, cool naturally to room temperature, an...

Embodiment 3

[0046] The nanometer electrode material LTO / TO-R that embodiment 1 and 2 obtains carries out XRD diffraction analysis and scanning electron microscope (SEM) morphology analysis, and the result is as follows figure 1 , image 3 shown.

[0047] figure 1 The XRD diffraction analysis spectrum of LTO / TO-R at different temperatures shows that the diffraction peaks of the samples calcined at 650-700°C ( figure 1 (b)) is consistent with LTO, TO-R standard cards; and the sample after calcining at 550-600 ° C is analyzed by XRD diffraction spectrum ( figure 1 (a) shows that in addition to the diffraction peaks of LTO and TO-R, anatase TiO also appeared 2 (TO-A) impurity peak; figure 1 In (a) and figure 1 The comparison in (b) shows that the XRD diffraction peaks of the sample LTO / TO-R calcined at 650-700°C are sharper, and the purity and crystallinity are higher.

[0048] Depend on image 3 (b) It can be seen that the target product LTO / TO-R obtained after calcination at 650-700°...

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Abstract

The invention discloses a composite solvothermal method for preparing nanometer electrode material Li 4 Ti 5 o 12 / Rutil‑TiO 2 Methods. Dissolve tetrabutyl titanate in a diethylene glycol aqueous solution, and stir it magnetically to make it evenly mixed to obtain a mixed solution; add lithium hydroxide aqueous solution to the obtained mixed solution, stir for 5-6 hours, and transfer the reaction solution to In a stainless steel autoclave, keep at 180°C for 35-40h, centrifuge to collect the precipitate, and dry it in an oven at 80°C to obtain a precursor; place the obtained precursor in a muffle furnace, and heat it at 550-700 ℃ calcined for 6-7 hours, naturally cooled to room temperature, and ground to obtain the target product Li 4 Ti 5 o 12 / Rutil‑TiO 2 . The invention adopts a simple and easy-to-operate solvothermal method for one-step synthesis, which is beneficial to realize the commercialization of LTO / TO-R nanometer electrode materials, and promotes the faster development of lithium-ion battery negative electrode materials.

Description

technical field [0001] The invention relates to the technical field of lithium ion batteries, in particular to a nano-electrode material lithium titanate Li prepared by a composite solvothermal method. 4 Ti 5 o 12 / Rutile-TiO 2 Methods. Background technique [0002] In recent years, due to the massive consumption of non-renewable resources such as coal and oil and environmental pollution, the development and marketization of electric vehicles and hybrid vehicles has become the focus of attention. The power supply is a key factor restricting the application of electric vehicles and hybrid vehicles. Among many types of batteries, lithium-ion batteries have attracted widespread attention due to their excellent performance. [0003] At present, small lithium-ion batteries with carbonaceous materials as negative electrodes have been widely used in small digital electronic products such as mobile phones, digital cameras and notebook computers. However, due to the rapid charge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/36H01M4/48H01M4/485H01M10/0525B82Y30/00
CPCB82Y30/00H01M4/366H01M4/483H01M4/485H01M10/0525Y02E60/10
Inventor 葛昊朱帅孙志佳王登虎聂胜楠宋溪明
Owner LIAONING UNIVERSITY