Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor

A technology of titanate nanotubes and lithium halite titanate, which is applied in the field of nanomaterial preparation technology and energy, can solve the problems of complex process and no obvious improvement in the electrochemical performance of nano lithium titanate, and achieve simple equipment and easy large-scale industrialization Production, fast results

Inactive Publication Date: 2006-01-25
TSINGHUA UNIV
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Problems solved by technology

[0005] High-energy ball milling method: Zaghib et al. used high-energy ball milling to pulverize ordinary micron-sized lithium titanate into nano-scale, and its particle size is about 600nm. However, the electrochemical performance of nano-lithium titanate prepared by this method is not good. no significant improvement
[0006] Sol-gel method: Gratzel et al. used stoichiometric titanium and lithium organic alkoxides as precursors to prepare spinel-type nano-lithium titanate through hydrolysis and sol-gel processes. Nano-lithium titanate shows excellent fast charge and discharge capabilities, even at a discharge rate of 250C, it also maintains a high capacity, but the sol-gel method requires expensive organic alkoxides as precursors, and the process is complex , so it is difficult to achieve large-scale industrial production to meet the large demand in the energy field

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  • Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor
  • Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor
  • Preparation method of spinel lithium titanate nano tube/wire for lithium battery and capacitor

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preparation example Construction

[0026] Preparation technique of the present invention mainly comprises following two aspects:

[0027] 1. Preparation of titanate nanotubes / nanowires from industrially produced titanium dioxide

[0028] This method of preparing titanate nanotubes / nanowires fully utilizes the pulverization effect of ultrasonic waves to fully pulverize large particle materials into fine particles, increases the contact area between materials, and reduces the mass transfer resistance of the reaction; The instantaneous local ultra-high temperature and ultra-high pressure generated by the chemical reaction accelerates the reaction, and then crystallizes by low-temperature hydrothermal to obtain titanate nanotubes / nanowires. After post-treatment, titanate nanotubes / nanowires are formed.

[0029] Process steps: Mix 1-5 grams of industrially produced titanium dioxide with 40 ml of 5-25 mol / liter NaOH solution, place in an ultrasonic generator, and perform ultrasonic chemical reaction at a temperature...

Embodiment 1

[0034] Embodiment 1: Preparation of titanate nanotubes

[0035] Weigh 1 g, 1.5 g, and 2.5 g of industrially produced anatase or rutile crystal form titanium dioxide powder, put them into a Erlenmeyer flask, add 40 ml of NaOH solution with a concentration of 5 or 10 mol / liter, and put them into an ultrasonic Generator, at 0.5W / cm 2 Ultrasonic with high power for 2 hours at a temperature of 30-80°C. Then move it into a 40ml polytetrafluoroethylene-lined autoclave, conduct a hydrothermal reaction at 110-120°C for 20 hours, centrifuge the white product from excess alkali, and use 0.1 mol / liter of HNO 3 Neutralize until the pH value is 3-7, age for 8 hours, rinse with deionized water, exchange with absolute ethanol three times, and dry to obtain titanate nanotubes. Its molecular formula is H 2 Ti 3 o 7 .

[0036] Repeat the above steps to 100W / cm 2 Ultrasound at a high power for 0.2 hours at a temperature of 60-80° C. to obtain titanate nanotubes.

[0037] The above operati...

Embodiment 2

[0040] Embodiment 2: Preparation of titanic acid nanowires

[0041] Weigh 3 grams, 4 grams or 5 grams of industrially produced titanium dioxide powder of anatase or rutile crystal form, put it into a Erlenmeyer flask, add 40 milliliters of NaOH solution with a concentration of 20 or 25 mol / liter, and put it into Ultrasonic generator, at 0.5W / cm 2 Ultrasonic with high power for 2 hours at a temperature of 30-80°C. Then move it into a 40ml polytetrafluoroethylene-lined autoclave, conduct a hydrothermal reaction at 170-180°C for 48 hours, centrifuge the white product from excess alkali, and use 0.1 mol / liter of HNO 3 Neutralize until the pH value is 5-7, age for 8 hours, then rinse with deionized water, exchange with absolute ethanol three times, and dry to obtain titanate nanowires; its molecular formula is H 2 Ti 3 o 7 .

[0042] Repeat the above steps to 100W / cm 2 Ultrasonic with high power for 0.5 hours at a temperature of 60-80° C. to obtain titanic acid nanowires.

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Abstract

This invention discloses a preparation method for spinel lithium titanate nm pipes/nm lines used in Li batteries and capacitors, which applies cheap industrial TiO2 as the raw material and supersonic chemical method to prepare said nm pipes/lines then takes them as the raw materials to be mixed with a certain quantity of soluble Li salt solution to be baked in air and by low-temperature hydrothermal ion exchange method to manufacture spinel lithium titanate nm pipes/lines with uniform shape, uniform diameter and even larger major diameter ratio and big ratio surface area.

Description

technical field [0001] The invention belongs to the field of nano material preparation technology and energy. In particular, it relates to methods of preparing spinel lithium titanate nanotubes / wires for lithium batteries and capacitors. technical background [0002] In recent years, spinel-type lithium titanate has been paid more and more attention as an electrode material for new energy storage batteries. This is because the lattice constant of spinel-type lithium titanate changes little before and after lithium ion insertion and extraction, which is called lithium The "zero-strain material" with ion intercalation can therefore have excellent cycle stability. At the same time, lithium titanate also has the characteristics of anti-overcharge performance, good thermal stability, high safety and large specific capacity. It is an excellent New battery materials are widely used in the field of energy storage batteries. Lithium titanate has a relatively low potential relative ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M4/04H01M4/58H01M4/48C01D15/00C01G23/00B82B3/00H01M4/485
CPCY02E60/12Y02E60/10
Inventor 唐子龙李俊荣张中太
Owner TSINGHUA UNIV
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