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Titanium oxide nano tube and preparing method thereof

A titanium oxide, titanate nanotube technology, applied in the direction of titanium oxide/hydroxide, titanium dioxide, etc., can solve the problems of thick nanotube diameter, harsh condition control requirements, harsh condition control, etc., and achieve easy large-scale industrial production. , the speed environment is friendly, the conditions are easy to control the effect

Inactive Publication Date: 2004-09-15
TSINGHUA UNIV
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Problems solved by technology

Synthesis of TiO by Template Method 2 The morphology of nanotubes is directly affected by the uniformity and thickness of the pore structure of the template. At the same time, the synthesis process also has a great influence on the product, and the condition control requirements are relatively strict. For example, the morphology of the product is very sensitive to the time of impregnation. To obtain Nanotubes, the impregnation time is very short, usually a few seconds, so it is difficult to achieve industrial mass production
The shorter the immersion time, the thinner the tube wall obtained, and the longer the immersion time, only nanowires can be obtained, and the obtained nanotubes are usually amorphous TiO 2 , and the tube wall is usually composed of nanoparticles, due to the limitation of the template, the diameter of the nanotube is relatively large, and the specific surface area is relatively small, and the sol-gel method usually requires expensive organic alkoxides as raw materials. High cost, not suitable for mass production
[0006] Organogel method: M.Adachi et al. used organic alkoxides of titanium as raw materials and organic ammonium surfactants as templates to synthesize TiO through a sol-gel process. 2 Nanotubes (Chemistry Letters, Chemistry Letters, 2000, page 942), the process of this method is more complicated, and the condition control is harsher, and the nanotubes prepared are usually amorphous structures, and the raw materials used are mostly organic matter, and are more expensive, so it is not suitable for mass production
[0007] Electrochemical anodic oxidation method: Recently, the Journal of Materials Research (Journal of Materials Research, 2001, Volume 16, page 3331) reported the preparation of TiO by electrochemical anodic oxidation 2 Nanotube arrays are used for gas-sensing or humidity-sensing elements. The diameter of the prepared nanotubes is relatively thick, and the tube walls are made of nano-TiO 2 Particle composition, the specific surface area is relatively small, which limits its application field

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  • Titanium oxide nano tube and preparing method thereof

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preparation example Construction

[0027] Preparation technique of the present invention mainly comprises following two aspects:

[0028] 1. Preparation of titanate nanotubes from industrially produced titanium dioxide

[0029] This method of preparing titanate nanotubes 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; at the same time, it uses ultrasonic cavitation to generate The instantaneous local ultra-high temperature and ultra-high pressure accelerate the reaction, and then use low-temperature hydrothermal crystallization to obtain titanate nanotubes. After post-treatment, titanate nanotubes are formed.

[0030] Process steps: mix 1-5 grams of industrially produced titanium dioxide with 40 ml of 5-20 mol / L NaOH solution, place in an ultrasonic generator, and perform ultrasonic chemical reaction at a temperature of 30-90°C and ...

Embodiment 1

[0036] Preparation of titanate nanotubes

[0037] Weigh 1.0 g of industrially produced anatase crystal form titanium dioxide powder, put it into an Erlenmeyer flask, add 40 ml of 10 mol / L NaOH solution, put it into an ultrasonic generator, and the ultrasonic temperature is 35 ° C, with 0.2 W / cm 2The power of ultrasound for 5 hours. Then move it into a 50mL polytetrafluoroethylene-lined autoclave, conduct a hydrothermal reaction at 125°C for 20 hours, centrifuge the white product from excess alkali, and use 0.1 mol / L of HNO 3 Neutralize until the pH value is 2-6, age, 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 ·H2O.

[0038] Repeat the above operation steps, the ultrasonic temperature is 85°C, and the ultrasonic temperature is 0.2W / cm 2 Ultrasound with high power for 2 hours can obtain titanate nanotubes.

[0039] Repeat the above operation steps, the ultrasonic tempe...

Embodiment 2

[0048] Weigh 1.0 g of industrially produced titanium dioxide powder of rutile crystal form, put it into an Erlenmeyer flask, add 40 milliliters of 10 mol / liter NaOH solution, put it into an ultrasonic generator, and use 0.2W / cm 2 Sonicate for 5 hours at a power of 85 °C. Then move it into a 50mL polytetrafluoroethylene-lined autoclave, conduct a hydrothermal reaction at 125°C for 30 hours, centrifuge the white product from excess alkali, and use 0.1 mol / L 3 Neutralize until the pH value is 2-6, 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 ·H2O.

[0049] Repeat the above operation steps, the ultrasonic temperature is 85°C, and the ultrasonic temperature is 0.2W / cm 2 Ultrasound with high power for 3 hours can obtain titanate nanotubes.

[0050] Repeat the above operation steps, the ultrasonic temperature is 35°C, and the ultrasonic temperature is 95W / cm ...

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Abstract

The invention relates to a Ti oxide nano tube and preparing method. Its character: using TiO2 of various crystal shapes as raw material, and making ultrasonic processing, hydrothermal reaction and after treatment in NaOH solution to obtain titanic acid nano tube, and then baking to form TiO2 nano tube with anatase structure. The TiO2 nano tube has uniform appearance, small tube diameter and large specific surface area. It has wide applied prospect in the fields of photocatalysis, environmental purification, solar cell, gas and wet sensitive materials, etc. It has low energy consumption, simple device, and easy controlled condition, easy to realize large-scale industrial production.

Description

technical field [0001] The invention relates to a titanium oxide nanotube and a preparation method thereof, belonging to the technical field of nanomaterial preparation. Background technique [0002] In 1991, Japanese scientist Iijima discovered carbon nanotubes. Due to their special chemical, physical and mechanical properties, carbon nanotubes have attracted the attention of scientists from all over the world. Carbon nanotubes usually need to be produced at high temperature. Following carbon nanotubes, nanomaterials with one-dimensional structures such as nanotubes, nanowires, and nanorods have become research hotspots. [0003] TiO 2 It is an oxide semiconductor material with a wide range of uses, and has broad application prospects in photocatalysis, environmental purification, catalyst carriers, lithium-ion batteries, gas sensors, and solar cells. TiO 2 There are three crystal forms, namely anatase, rutile and brookite. Due to TiO 2 Wide range of applications, peopl...

Claims

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Application Information

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IPC IPC(8): C01G23/047
Inventor 张中太李俊荣唐子龙
Owner TSINGHUA UNIV
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