Method for preparing doped nano titanium dioxide powder by microwave hydrothermal method

Abstract

The invention discloses a method for preparing doped nano titanium dioxide powder by a microwave hydrothermal method, wherein the method comprises the following steps: firstly, dropwise adding a InCl3.4H2O solution completely dissolved in absolute ethyl alcohol into a NbCl5 solution completely dissolved in absolute ethyl alcohol; then dropwise adding the obtained solution into a uniform mixed solution of absolute ethyl alcohol and tetrabutyl titanate; then dropwise adding concentrated hydrochloric acid to adjust the pH, and forming a (In0.05Nb0.05)Ti0.9O2 precursor solution; heating the (In0.05Nb0.05)Ti0.9O2 precursor solution by using a microwave hydrothermal system; and finally, cleaning powder obtained after the reaction with absolute ethyl alcohol, filtering and drying, to obtain a nano-sized (In0.05Nb0.05)Ti0.9O2 powder. The period of preparation of the powder by the microwave hydrothermal method is short, the purity of the product is high, and the crystal grain size can reach nano scale, so that the solution is evenly heated in a shorter time without temperature gradient or hysteresis effect; the nano (In0.05Nb0.05)Ti0.9O2 powder prepared by the method has the advantages of high purity, good dispersibility and uniform particle size distribution, and the particle size distribution is 700 nm-800 nm.

Description

technical field

[0001] The invention belongs to the field of preparing nano-powder by wet chemical method, and in particular relates to a method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method. Background technique

[0002] In recent years, modern communication technology, Internet, local area network and microelectronic technology have been continuously developed, and electronic technology has been widely used in national defense, science, industry, medicine, communication (information processing, transmission and communication), radio, television, aviation, navigation, radio Various fields such as positioning, automatic control, remote control and telemetry, computer and cultural life play an important role in promoting the development of the national economy. And with the development of electronic technology and industry, the development of microelectronic devices requires smaller volume, faster speed, higher frequency and lower power con...

Examples

Embodiment 1

[0031] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0032] Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0033] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0034] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0035] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D...

Embodiment 2

[0040] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0041] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 and InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0042] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0043] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D solution;

[0044] (4) Slowly drop the D solution obtained in the step (3) into the C solution, and continue stirring until a uniform mixed solution is obtained;

[0045] (5) Select concentrated hydrochloric acid to regulate the pH of the soluti...

Embodiment 3

[0048] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0049] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0050] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0051] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D solution;

[0052] (4) Slowly drop the D solution obtained in step (3) into the solution C, and keep stirring until a uniform mixed solution is obtained;

[0053] (5) select concentrated hydrochloric acid to regulate solution pH for use, slowly ad...

technical field

[0001] The invention belongs to the field of preparing nano-powder by wet chemical method, and in particular relates to a method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method. Background technique

[0002] In recent years, modern communication technology, Internet, local area network and microelectronic technology have been continuously developed, and electronic technology has been widely used in national defense, science, industry, medicine, communication (information processing, transmission and communication), radio, television, aviation, navigation, radio Various fields such as positioning, automatic control, remote control and telemetry, computer and cultural life play an important role in promoting the development of the national economy. And with the development of electronic technology and industry, the development of microelectronic devices requires smaller volume, faster speed, higher frequency and lower power con...

Examples

Embodiment 1

[0031] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0032] Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0033] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0034] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0035] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D...

Embodiment 2

[0040] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0041] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 and InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0042] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0043] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D solution;

[0044] (4) Slowly drop the D solution obtained in the step (3) into the C solution, and continue stirring until a uniform mixed solution is obtained;

[0045] (5) Select concentrated hydrochloric acid to regulate the pH of the soluti...

Embodiment 3

[0048] A method for preparing doped nano-titanium dioxide powder by microwave hydrothermal method, comprising the steps of:

[0049] (1) Accurately weigh NbCl according to the molar ratio of 1:1 5 , InCl 3 4H 2 O and add an appropriate amount of absolute ethanol and continue to stir to make it completely dissolved, respectively, to obtain uniform A solution and B solution.

[0050] (2) Measure tetra-n-butyl titanate and place it in a beaker, add an appropriate amount of absolute ethanol dropwise, and continue to stir to obtain a uniform C solution, wherein tetra-n-butyl titanate and NbCl in step (1) 5 The molar ratio is 18:1;

[0051] (3) Slowly drop the B solution into the A solution, and continue to stir evenly to obtain the D solution;

[0052] (4) Slowly drop the D solution obtained in step (3) into the solution C, and keep stirring until a uniform mixed solution is obtained;

[0053] (5) select concentrated hydrochloric acid to regulate solution pH for use, slowly ad...

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