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Hydrothermal preparation method of shape-controllable titanium dioxide nano tube

A technology of titanium dioxide and hydrothermal method, applied in the direction of titanium dioxide, titanium oxide/hydroxide, nanotechnology, etc., can solve the problems of controllability of nanotube morphology, achieve controllable length, high tube forming efficiency, The effect of uniform diameter

Inactive Publication Date: 2013-11-20
HARBIN ENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The patent document with the publication number CN101239738A discloses a preparation method of titanium dioxide nanotubes. Its main feature is that nanotubes with relatively uniform diameters are prepared, but the controllable shape of nanotubes is not realized.

Method used

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  • Hydrothermal preparation method of shape-controllable titanium dioxide nano tube
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  • Hydrothermal preparation method of shape-controllable titanium dioxide nano tube

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Step 1: Prepare 20 mL of NaOH solution with a concentration of 10 mol / L and add it to the reaction kettle.

[0024] Step 2, weighing 3g of anatase phase titanium dioxide nanopowder with a particle size of 15nm, adding it into the prepared concentrated alkali solution and ultrasonically vibrating to make it evenly mixed.

[0025] Step 3: Put the reactor into an oven for hydrothermal reaction at 130° C. for 30 hours.

[0026] Step 4: After the hydrothermal reaction is completed, the supernatant is poured out, and the obtained solid powder is washed with water until neutral.

[0027] Step five, adding 0.1 mol / L nitric acid or hydrochloric acid to the obtained powder, and ultrasonicating at 50-100° C. for 1-3 hours.

[0028] In step six, the acid-treated sample is washed with water until it is nearly neutral.

[0029] Step seven, filter.

[0030] Step eight, fully dry the obtained powder.

[0031] Step 9, calcining the dried powder at 400° C. for 2 hours.

Embodiment 2

[0033] Step 1: Prepare 20 mL of NaOH solution with a concentration of 10 mol / L and add it to the reaction kettle.

[0034] Step 2, weighing 0.05g of cetyltrimethylammonium bromide and 3g of anatase phase titanium dioxide nanopowder with a particle size of 15nm, adding them into the prepared concentrated alkali solution and ultrasonically vibrating to mix them evenly.

[0035] Step 3: Put the reactor into an oven for hydrothermal reaction at 130° C. for 30 hours.

[0036] Step 4: After the hydrothermal reaction is completed, the supernatant is poured out, and the obtained solid powder is washed with water until neutral.

[0037] Step five, adding 0.1 mol / L nitric acid or hydrochloric acid to the obtained powder, and ultrasonicating at 50-100° C. for 1-3 hours.

[0038] In step six, the acid-treated sample is washed with water until it is nearly neutral.

[0039] Step seven, filter.

[0040] Step eight, fully dry the obtained powder.

[0041] Step 9, calcining the dried powd...

Embodiment 3

[0043] Step 1: Prepare 20 mL of NaOH solution with a concentration of 10 mol / L and add it to the reaction kettle.

[0044] Step 2: Weigh 0.1 g of cetyltrimethylammonium bromide and 3 g of anatase phase titanium dioxide nanopowder with a particle size of 15 nm, and add them into the prepared concentrated alkali solution by ultrasonic vibration to mix them evenly.

[0045] Step 3: Put the reactor into an oven for hydrothermal reaction at 130° C. for 30 hours.

[0046] Step 4: After the hydrothermal reaction is completed, the supernatant is poured out, and the obtained solid powder is washed with water until neutral.

[0047] Step five, adding 0.1 mol / L nitric acid or hydrochloric acid to the obtained powder, and ultrasonicating at 50-100° C. for 1-3 hours.

[0048] In step six, the acid-treated sample is washed with water until it is nearly neutral.

[0049] Step seven, filter.

[0050] Step eight, fully dry the obtained powder.

[0051] Step 9, calcining the dried powder at...

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Abstract

The invention provides a hydrothermal preparation method of a shape-controllable titanium dioxide nano tube. The hydrothermal preparation method comprises the following steps of: adding 10-50mL of NaOH solution with the concentration being 8-15mol / L into a reaction kettle; then adding 0.1-10g of cetyl trimethyl ammonium bromide and 01-3g of titanium dioxide nano powder into the reaction kettle, and carrying out ultrasonic oscillation to mix the materials uniformly; carrying out hydrothermal reaction in the reaction kettle at the temperature of 100-200 DEG C for 15-30 hours; pouring out supernatant, and washing the obtained solid powder with water to be neutral; adding 0.1-1mol / L of nitric acid or hydrochloric acid into the obtained powder, carrying out ultrasonic oscillation for 1-3 hours at the temperature of 50-100 DEG C; washing a product (which is obtained after acid treatment) with water to be neutral nearly, filtering and drying; and calcining the dried powder for 1-5 hours at the temperature of 400-800 DEG C. The obtained titanium dioxide nano tube is influenced by the adding amount of a surface active agent, the length is controllable, the tube diameter is more uniform, the two ends are open, the tube forming efficiency is high, and therefore the titanium dioxide nano tube can be favorably applied to nanoscience, biomedicine and the like.

Description

technical field [0001] The invention relates to a preparation method of titanium dioxide nanotubes, in particular to a method for preparing morphology-controllable titanium dioxide nanotube powders by a hydrothermal method. Background technique [0002] Since Kasuga et al. prepared titanium dioxide nanotubes for the first time in 1998, this one-dimensional nanomaterial, which is non-toxic and harmless, has high chemical stability, and has many excellent properties such as gas sensitivity, catalytic activity, and photoelectric conversion effect, has attracted the attention of the scientific community. widespread attention. There are three main methods for preparing titanium dioxide nanotubes: hard template method, anodic oxidation method and hydrothermal method. Among them, the hydrothermal method has aroused great interest among scholars due to its simple operation process and high purity of the prepared titanium dioxide nanotubes. However, how to effectively control its m...

Claims

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Application Information

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IPC IPC(8): C01G23/053B82Y30/00
Inventor 董国君孙逍寒李茹民
Owner HARBIN ENG UNIV
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