A method for adjusting the length of tungsten oxide nanorods by oxygen

Abstract

The invention provides a method for adjusting the length of a tungsten oxide nano-rod by means of oxygen and belongs to the technical field of tungsten-based nano-materials. According to the method, tungsten metal salt serves as a tungsten source, a carbon nano-tube serves as a carrier, ethanediol serves as a dispersant, hydrochloric acid is added into the reaction system, tungstic acid is directly separated out of the surface of the carbon nano-tube and covers the surface of the carbon nano-tube, tungstic acid grows along the surface of the carbon nano-tube, and then a tungstic acid / carbon nano-tube rodlike composite is formed. Then, the composite is put in a high-temperature reaction region for heat treatment, an oxidizing atmosphere is introduced, the carbon nano-tube is burnt, the burning degree of the carbon nano-tube and the generation speed of carbon dioxide are controlled by controlling the gas flow and the oxygen content, the breakage degree and surface shrinkage degree of the tungsten oxide nano-rod are controlled accordingly, and therefore the purpose of shearing the tungsten oxide nano-rod is achieved.

Description

technical field

[0001] The invention relates to a preparation method in the technical field of tungsten-based nanomaterials, in particular to a method for adjusting the length of tungsten oxide nanorods by oxygen. Background technique

[0002] Tungsten oxide with nanostructure exhibits special physical effects due to its high specific surface area, which makes it have broad application value in the fields of electrochromism, photochromism, sensing and catalysis. The performance of tungsten carbide is mainly closely related to the raw material of tungsten oxide. During the carbonization and reduction process of tungsten oxide, the tungsten carbide grains formed are easy to form abnormally coarse particles due to mutual aggregation. Therefore, if nanostructured tungsten oxide with high specific surface area can be prepared, its physical and chemical properties will be further improved, and its application value will be expanded, especially its value in the field of preparation...

Examples

Embodiment 1

[0022]Soak 12 mg of carbon nanotubes with a diameter of 30-200 nm and a layer number of 20-30 in nitric acid, reflux at 100 °C under constant temperature stirring, and after drying, disperse in 100 mL of ethylene glycol and ultrasonically disperse for 24 hours. Obtain a uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL deionized water to obtain a clear sodium tungstate solution B with a concentration of 0.1 mol / L; solution Add B into solution A, and mix it uniformly under the action of a constant temperature magnetic stirrer, then add an appropriate amount of hydrochloric acid dropwise to adjust the pH value of the solution to 1; reflux for 10 h under the condition of a constant temperature oil bath at 140°C, Then carry out vacuum filtration and washing, the drying temperature is 110 ℃, and the holding time is 2 h; obtain the rod-shaped composite C of carbon nanotubes and tungstic ...

Embodiment 2

[0024] Soak 12 mg of carbon nanotubes with a diameter of 30-200 nm and a layer number of 20-30 in nitric acid, reflux at 100 °C under constant temperature stirring, dry and disperse in 100 mL of ethylene glycol, and ultrasonically disperse for 24 hours to obtain Uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL deionized water to obtain a clear sodium tungstate solution B with a concentration of 0.1 mol / L; solution B Add it into solution A, mix it evenly under the action of a constant temperature magnetic stirrer, then add an appropriate amount of hydrochloric acid dropwise to it, and adjust the pH value of the solution to 1; reflux for 10 h under the condition of a constant temperature oil bath at 140 °C, and then Vacuum filtration and washing were carried out, the drying temperature was 110 °C, and the holding time was 2 h; the rod-shaped composite C of carbon nanotubes and tungs...

Embodiment 3

[0026] Soak 12 mg of carbon nanotubes with a diameter of 15-150 nm and layers of 10-20 layers in nitric acid, reflux at 130 °C under constant temperature stirring, dry, disperse in 100 mL of ethylene glycol, and ultrasonically disperse for 24 hours to obtain Uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL of deionized water and ethylene glycol mixture to obtain a clear concentration of 0.2 mol / L tungsten Sodium acid solution B; solution B is added to solution A, under the action of ultrasonic waves, mix it evenly, and then add an appropriate amount of hydrochloric acid to it, and adjust the pH value of the solution to 3; reflux under the condition of a constant temperature oil bath at 120°C 6 h, then carry out vacuum filtration and washing, the drying temperature is 100 ℃, and the holding time is 2 h; obtain the rod-shaped composite C of carbon nanotubes and tungstic acid; spread...

technical field

[0001] The invention relates to a preparation method in the technical field of tungsten-based nanomaterials, in particular to a method for adjusting the length of tungsten oxide nanorods by oxygen. Background technique

[0002] Tungsten oxide with nanostructure exhibits special physical effects due to its high specific surface area, which makes it have broad application value in the fields of electrochromism, photochromism, sensing and catalysis. The performance of tungsten carbide is mainly closely related to the raw material of tungsten oxide. During the carbonization and reduction process of tungsten oxide, the tungsten carbide grains formed are easy to form abnormally coarse particles due to mutual aggregation. Therefore, if nanostructured tungsten oxide with high specific surface area can be prepared, its physical and chemical properties will be further improved, and its application value will be expanded, especially its value in the field of preparation...

Examples

Embodiment 1

[0022]Soak 12 mg of carbon nanotubes with a diameter of 30-200 nm and a layer number of 20-30 in nitric acid, reflux at 100 °C under constant temperature stirring, and after drying, disperse in 100 mL of ethylene glycol and ultrasonically disperse for 24 hours. Obtain a uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL deionized water to obtain a clear sodium tungstate solution B with a concentration of 0.1 mol / L; solution Add B into solution A, and mix it uniformly under the action of a constant temperature magnetic stirrer, then add an appropriate amount of hydrochloric acid dropwise to adjust the pH value of the solution to 1; reflux for 10 h under the condition of a constant temperature oil bath at 140°C, Then carry out vacuum filtration and washing, the drying temperature is 110 ℃, and the holding time is 2 h; obtain the rod-shaped composite C of carbon nanotubes and tungstic ...

Embodiment 2

[0024] Soak 12 mg of carbon nanotubes with a diameter of 30-200 nm and a layer number of 20-30 in nitric acid, reflux at 100 °C under constant temperature stirring, dry and disperse in 100 mL of ethylene glycol, and ultrasonically disperse for 24 hours to obtain Uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL deionized water to obtain a clear sodium tungstate solution B with a concentration of 0.1 mol / L; solution B Add it into solution A, mix it evenly under the action of a constant temperature magnetic stirrer, then add an appropriate amount of hydrochloric acid dropwise to it, and adjust the pH value of the solution to 1; reflux for 10 h under the condition of a constant temperature oil bath at 140 °C, and then Vacuum filtration and washing were carried out, the drying temperature was 110 °C, and the holding time was 2 h; the rod-shaped composite C of carbon nanotubes and tungs...

Embodiment 3

[0026] Soak 12 mg of carbon nanotubes with a diameter of 15-150 nm and layers of 10-20 layers in nitric acid, reflux at 130 °C under constant temperature stirring, dry, disperse in 100 mL of ethylene glycol, and ultrasonically disperse for 24 hours to obtain Uniformly dispersed carbon nanotube ethylene glycol suspension A with a concentration of 0.01 mol / L; completely dissolve sodium tungstate in 100 mL of deionized water and ethylene glycol mixture to obtain a clear concentration of 0.2 mol / L tungsten Sodium acid solution B; solution B is added to solution A, under the action of ultrasonic waves, mix it evenly, and then add an appropriate amount of hydrochloric acid to it, and adjust the pH value of the solution to 3; reflux under the condition of a constant temperature oil bath at 120°C 6 h, then carry out vacuum filtration and washing, the drying temperature is 100 ℃, and the holding time is 2 h; obtain the rod-shaped composite C of carbon nanotubes and tungstic acid; spread...

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