Preparation method of silver filled titanium dioxide nanometer tubes

A technology of titanium dioxide and nanotubes, which is applied in the field of nanomaterials and can solve problems such as the difficulty in filling precious metal silver nanoparticles

Active Publication Date: 2018-08-10

芜湖启博知识产权运营有限公司

2 Cites 0 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Titanium dioxide nanotubes prepared by hydrothermal method have the characteristics of thin tube wall, high aspect ratio and large specific surface, but because the tube diam...

Abstract

The invention discloses a preparation method of silver filled titanium dioxide nanometer tubes. According to the method, a hydrothermal method is used for preparing titanium dioxide nanometer tubes; titanium dioxide nanometer tube particles are put into a tubular furnace; then, N2 is charged into the boiling CCl4 liquid; the generated mixed gas is guided into the tubular furnace; the nanometer silver is filled into the defect titanium dioxide nanometer tubes. According to the method, CCl4 is used for etching the titanium dioxide nanometer tubes; hollow hole defects are formed in the titanium dioxide nanometer tubes. The filling of the nanometer silver in the titanium dioxide nanometer tubes can be facilitated; the silver filled titanium dioxide nanometer tube material is obtained.

Application Domain

Material nanotechnologyCatalyst activation/preparation +1

Technology Topic

Tube furnaceTitanium dioxide +4

Examples

Experimental program(4)
Comparison scheme(1)
Effect test(1)

Example Embodiment

[0019] Example 1:

[0020] Step (1). Using hydrothermal method to prepare titanium dioxide nanotubes:

[0021] Add Degussa P-25 titanium dioxide nanoparticles into a plastic container containing a 10M sodium hydroxide aqueous solution, stir and disperse, and then transfer to a stainless steel reactor lined with polytetrafluoroethylene material for reaction. The reaction temperature is 100°C. , The reaction time is 30 hours; after the reaction is completed, cool to room temperature, filter the precipitate, wash with deionized water, and calcinate in a muffle furnace at 400°C for 4 hours. Then, place it in a 0.1M dilute nitric acid aqueous solution and soak for 12 hours, then wash with deionized water to the solution pH=7, and dry it in an oven to obtain titanium dioxide nanotube particles;

[0022] Step (2). Formation of titanium dioxide nanotube defects:

[0023] Place the titanium dioxide nanotube particles in a tube furnace, and then in the boiling CCl 4 Fill the liquid with N 2 , The mixed gas produced is introduced into the tube furnace. N 2 The flow rate is 5ml/min, the temperature of the tube furnace is controlled at 600°C, and the time is 2 hours.

[0024] Step (3). Nano-silver filled titanium dioxide nanotubes:

[0025] Change 0.5ml concentration to 0.1mol/LAgNO 3 The aqueous solution and 0.1ml of 0.5mol/L alkaline NaOH aqueous solution were added to 25ml of ethylene glycol. Then add 0.05 g of defective titanium dioxide nanotube particles and stir for 4 hours under vacuum. After stirring, the mixed solution was heated in a microwave oven (2450MHZ, 700W) for 30s, filtered and washed with acetone, and dried to obtain silver-filled titanium dioxide nanotube material.

Example Embodiment

[0026] Example 2:

[0027] Step (1). Using hydrothermal method to prepare titanium dioxide nanotubes:

[0028] Add Degussa P-25 titanium dioxide nanoparticles into a plastic container containing 15M sodium hydroxide aqueous solution, stir and disperse, and then transfer to a stainless steel reactor lined with polytetrafluoroethylene material for reaction. The reaction temperature is 140°C. , The reaction time is 15 hours; after the reaction, it is cooled to normal temperature, the precipitate is filtered, washed with deionized water, and calcined in a muffle furnace at 500°C for 2 hours. Then, place it in 0.1M dilute nitric acid aqueous solution to soak for 24 hours, and then wash with deionized water to the solution pH=7, and dry in an oven to obtain titanium dioxide nanotube particles;

[0029] Step (2). Formation of titanium dioxide nanotube defects:

[0030] Place the titanium dioxide nanotube particles in a tube furnace, and then in the boiling CCl 4 Fill the liquid with N 2 , The mixed gas produced is introduced into the tube furnace. N 2 The flow rate of the tube furnace is 20ml/min, the temperature of the tube furnace is controlled at 400°C, and the time is 0.5 hours.

[0031] Step (3). Nano-silver filled titanium dioxide nanotubes:

[0032] Set the concentration of 1ml to 0.01mol/LAgNO 3 The aqueous solution and 0.5 ml of alkaline KOH aqueous solution with a concentration of 0.1 mol/L were added to 25 ml of ethylene glycol. Then, 0.1 g of defective titanium dioxide nanotube particles were added and stirred for 2 hours under vacuum. After stirring, the mixed solution was heated in a microwave oven (2450MHZ, 700W) for 60s, filtered and washed with acetone, and dried to obtain silver-filled titanium dioxide nanotube material.

Example Embodiment

[0033] Example 3:

[0034] Step (1). Using hydrothermal method to prepare titanium dioxide nanotubes:

[0035] Add Degussa P-25 titanium dioxide nanoparticles into a plastic container with a concentration of 12M sodium hydroxide aqueous solution, stir and disperse, and then transfer to a stainless steel reactor lined with polytetrafluoroethylene material for reaction. The reaction temperature is 120°C. , The reaction time is 20 hours; after the reaction, it is cooled to normal temperature, the precipitate is filtered, washed with deionized water, and calcined in a muffle furnace at 450°C for 3 hours. Then, place it in a 0.1M dilute nitric acid aqueous solution to soak for 18 hours, then wash with deionized water to the solution pH=7, and dry in an oven to obtain titanium dioxide nanotube particles;

[0036] Step (2). Formation of titanium dioxide nanotube defects:

[0037] Place the titanium dioxide nanotube particles in a tube furnace, and then in the boiling CCl 4 Fill the liquid with N 2 , The mixed gas produced is introduced into the tube furnace. N 2 The flow rate of the tube furnace is 10ml/min, the temperature of the tube furnace is controlled at 500°C, and the time is 1 hour.

[0038] Step (3). Nano-silver filled titanium dioxide nanotubes:

[0039] Set 0.8ml concentration to 0.05mol/LAgNO 3 The aqueous solution and 0.3ml of a 0.3mol/L alkaline NaOH and KOH mixed aqueous solution (1:1) were added to 25ml of ethylene glycol. Then add 0.08 g of defective titanium dioxide nanotube particles, and stir for 3 hours under vacuum. After stirring, the mixture was heated in a microwave oven (2450MHZ, 700W) for 50s, filtered and washed with acetone, and dried to obtain silver-filled titanium dioxide nanotube material.

PUM

Description & Claims & Application Information

We can also present the details of the Description, Claims and Application information to help users get a comprehensive understanding of the technical details of the patent, such as background art, summary of invention, brief description of drawings, description of embodiments, and other original content. On the other hand, users can also determine the specific scope of protection of the technology through the list of claims; as well as understand the changes in the life cycle of the technology with the presentation of the patent timeline. Login to view more.