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A kind of preparation method of titanium dioxide nanotube doped with asymmetric metal salt

A technology of titanium dioxide and metal salts, applied in the field of preparation of titanium dioxide nanotubes, can solve the problems of long hydrothermal time, multiple energy sources, high cost, etc., and achieve the effect of small particle size and high specific surface area

Inactive Publication Date: 2015-08-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing research is mainly on high-cost titanium dioxide P25 powder, and the preparation of synthetic pure phase TiO 2 Nanotube structure, long hydrothermal time, consumes more energy. There are few reports about the one-pot precipitation of titanium ester compounds and doped raw materials-hydrothermal preparation of nanotubes, which can improve the negative electrode rate and cycle performance of lithium-ion batteries.

Method used

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  • A kind of preparation method of titanium dioxide nanotube doped with asymmetric metal salt
  • A kind of preparation method of titanium dioxide nanotube doped with asymmetric metal salt
  • A kind of preparation method of titanium dioxide nanotube doped with asymmetric metal salt

Examples

Experimental program
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Effect test

Embodiment 1

[0038] 0.6g Fe(NO 3 ) 3 Dissolve in 35mL of absolute ethanol, then add 10mL of titanium tetrachloride to the above salt solution, stir for 30min and mix well. Then, 100 mL of ammonia aqueous solution with a mass fraction of 3 to 6% was added to the solution while stirring to obtain a light yellow suspension, and the stirring was continued for 2.5 h. The light yellow suspension and the light yellow precipitate after centrifugation were washed several times with absolute ethanol, and then vacuum dried at 70°C for 2.5 hours.

[0039] 0.6 g of the dried powdery solid was weighed and added to 60 mL of NaOH solution with a concentration of 9 mol, followed by magnetic stirring for 30 min, and the mixed solution was transferred to the reaction kettle. The sealed reaction kettle was placed in an oven, heated to 150°C, and kept for 24h. When the temperature of the reactor was lowered to room temperature, the supernatant was poured out, and the light yellow precipitate at the bottom was...

Embodiment 2

[0041] Dissolve 0.55 g of zinc acetate in 40 mL of absolute ethanol, then add 11 mL of titanium tetrachloride to the above salt solution, stir for 30 min and mix well. Then, an aqueous ammonia solution with a mass fraction of 5-7% was added to the solution while stirring to obtain a light blue suspension, and the stirring was continued for 2.5 h. The blue suspension and the white precipitate after centrifugation were washed several times with absolute ethanol, and then vacuum dried at 70°C for 2.5h.

[0042] 0.6 g of the dried powdery solid was weighed and added to 60 mL of NaOH solution with a concentration of 10 mol / L, followed by magnetic stirring for 40 min, and the mixed solution was transferred to the reaction kettle. The sealed reaction kettle was placed in an oven, heated to 135°C, and kept for 72h. When the temperature of the reactor was lowered to room temperature, the supernatant was poured out, and the light blue precipitate at the bottom was washed with deionized...

Embodiment 3

[0045] Dissolve 1.0 g of lanthanum acetate in 50 mL of absolute ethanol, then add 10 mL of tetra-n-butyl titanate to the above salt solution, and stir for 30 min to mix well. Then, 5-7% ammonia aqueous solution was added to the solution while stirring to obtain a white suspension, and the stirring was continued for 2.5 h. The white suspension and the white precipitate after centrifugation were washed several times with absolute ethanol, and then vacuum-dried at 70°C for 2.5 hours.

[0046] 0.8 g of the dried powdered solid was weighed and added to 80 mL of NaOH solution with a concentration of 11 mol, followed by magnetic stirring for 30 min, and the mixed solution was transferred to the reaction kettle. The sealed reaction kettle was placed in an oven, heated to 120°C, and kept for 72h. When the temperature of the reactor was lowered to room temperature, the supernatant was poured out, and the white precipitate at the bottom was washed with deionized water while ultrasonicat...

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Abstract

The invention relates to a preparation method of a titanium dioxide nano tube doped with a heterovalent metal salt. The method comprises the following steps: firstly, selecting certain titanium source and doped metal salt to dissolve in an alcoholic solution together, and then adding a certain amount of weak alkali ammonia water, so as to obtain white sediments; transferring to a reaction kettle after washing and drying, so as to obtain the doped titanium dioxide nano tube by controlling the reaction temperature and time. The doped titanium dioxide nano tube prepared by the method is low in cost and simple in method; the transmission path of lithium ions can be shortened by applying the method to a lithium-ion battery; the rate capability of the lithium-ion battery is effectively improved; the cyclic capacity retention ratio of the battery is increased.

Description

technical field [0001] The invention belongs to the field of material chemistry lithium ion batteries, and in particular relates to a preparation method of a titanium dioxide nanotube doped with a heterovalent metal salt applied to a lithium ion battery. Background technique [0002] The volume expansion rate of titanium metal oxide is small, and the discharge platform is higher than that of graphite negative electrode, which can avoid the precipitation of metal lithium, and is a safe low-voltage battery material. Nanomaterials of TiO2 with different morphologies have attracted extensive attention due to their good performance of lithium deintercalation. Moreover, the nanostructure of one-dimensional titanium oxide has a large specific surface area and is rich in surface defects, which shortens the diffusion path of lithium ions in the electrochemical deintercalation process of lithium ions in space, which can be beneficial to the realization of fast charging and fast discha...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M4/48H01M4/62B82Y30/00
CPCB82Y40/00H01M4/362H01M4/48H01M4/626H01M10/0525Y02E60/10
Inventor 张建新路婷婷丁昭郡冯小钰姚斌
Owner SHANDONG UNIV
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