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Preparation method of conductive metal doped metallic oxide nano particles

A technology of conductive metals and nanoparticles, applied in the direction of material analysis, measuring devices, instruments, etc. through electromagnetic means, can solve problems such as high risk, prone to accidents, and threats to the safety of operators, so as to improve detection performance and shorten Preparation time, the effect of improving electron transfer efficiency

Inactive Publication Date: 2014-07-23
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the biggest disadvantage of this method is that it uses explosive and flammable raw materials such as ammonium nitrate and nitroglycerin. During the operation, especially when burning, if the experimental conditions are not well controlled, accidents are prone to occur, which poses a safety threat to operators. higher sex

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A preparation method of niobium, vanadium doped titanium dioxide nanoparticles, comprising the following steps:

[0031] 1) Prepare complexing agent solution.

[0032] Weigh 6.0g (0.0286mol) of citric acid monohydrate, add it to a beaker containing 200ml deionized water, heat and stir at 80°C until the citric acid is fully dissolved.

[0033] 2) Acidification.

[0034] In the above complexing agent solution, add 5ml of concentrated nitric acid (mass fraction is about 65%, density is about 1.4g / cm 3 ).

[0035] 3) Add metal oxide raw materials.

[0036] Accurately measure 35ml of tetrabutyl titanate (equivalent to 0.1mol of titanium dioxide), slowly drop into the solution, and keep stirring at 90°C for about 2h until the solution becomes clear.

[0037] 4) Adjust the pH.

[0038] Keeping the temperature and stirring conditions constant, a certain amount of ammonia water was added dropwise to the solution until the pH of the solution was 7.0.

[0039] 5) Add the sol...

Embodiment 2

[0051] A method for preparing niobium-doped titanium dioxide nanoparticles, comprising the following steps:

[0052] 1) Prepare complexing agent solution.

[0053] Weigh 2.10g (0.01mol) of citric acid monohydrate, add it to a beaker containing 100ml deionized water, heat and stir at 60°C until the citric acid is fully dissolved.

[0054] 2) Acidification.

[0055] In the above complexing agent solution, add 3.3ml of concentrated nitric acid (mass fraction is about 65%, density is about 1.4g / cm 3 ).

[0056] 3) Add metal oxide raw materials.

[0057] Accurately measure 35ml of tetrabutyl titanate (equivalent to 0.1mol of titanium dioxide), slowly drop into the solution, and keep stirring at 80°C for about 2h until the solution becomes clear.

[0058] 4) Adjust the pH.

[0059] Keeping the temperature and stirring conditions constant, a certain amount of ammonia water was added dropwise to the solution until the pH of the solution was 7.5.

[0060] 5) Add the soluble salt ...

Embodiment 3

[0071] A preparation method of vanadium-doped titanium dioxide nanoparticles, comprising the following steps:

[0072] 1) Prepare complexing agent solution.

[0073] Weigh 0.186g (0.0005mol) of disodium ethylenediaminetetraacetic acid (EDTA), add it into a beaker containing 11ml of deionized water, heat and stir at 100°C until the disodium ethylenediaminetetraacetic acid is fully dissolved.

[0074] 2) Acidification.

[0075] In the above complexing agent solution, add 0.22ml of concentrated nitric acid (mass fraction is about 65%, density is about 1.4g / cm 3 ).

[0076] 3) Add metal oxide raw materials.

[0077] Accurately measure 35 ml of tetrabutyl titanate (equivalent to 0.1 mol of titanium dioxide), slowly drop into the solution, and keep stirring at 100° C. for about 1 h until the solution becomes clear.

[0078] 4) Adjust the pH.

[0079] Keeping the temperature and stirring conditions constant, a certain amount of ammonia water was added dropwise to the solution un...

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Abstract

The invention discloses a preparation method of conductive metal doped metallic oxide nano particles, belonging to the technical field of nano particle preparation. The method comprises the following steps: (1) preparing a complexing agent solution; (2) acidifying; (3) adding with a metallic oxide raw material; (4) regulating pH value; (5) adding conductive metal soluble salt; (6) baking; and (7) decarbonizing. According to the method, appropriate amounts of concentrated nitric acid and ammonium hydroxide are added to well control hydrolysis of the metallic oxide raw material in solution, and the complexing property of the complexing agent to metal ions is utilized to perform complexation on conductive metal in conductive metal soluble salt, and the reaction is carried out slowly at high temperature, and therefore, the conductive metal doped metallic oxide nano particles are prepared; the method has the advantage of simplicity and convenience in operation, and the prepared nano particles have the characteristics of small particle size, good uniformity and good doping effect.

Description

technical field [0001] The invention relates to a method for preparing nanoparticles, in particular to a method for preparing conductive metal-doped metal oxide nanoparticles. Background technique [0002] In conventional techniques, doped metal oxide materials (such as niobium-doped titanium dioxide, etc.) are usually synthesized by a solid-phase method, a liquid-phase method or a combustion method. [0003] Solid-phase synthesis has the advantage of a large amount of synthetic products, but it also has the problem of high phase formation temperature, usually higher than 1000°C, and the preparation process requires multiple tableting and grinding, and the synthesis time is long, usually greater than 24 hours. Moreover, the synthesized product has large particles, the particle size is difficult to be uniform, and the doping efficiency is not ideal. [0004] The advantage of the liquid phase method is that nanoparticles with uniform and controllable particle size can be prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/327
Inventor 梁德沛李核刘付建谭婉琪王力清陈纪文陈卓梅王娜冯艳陈丹玲沈宏林陈满英李衍春佘之蕴周桂萍李薇
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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