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Preparation method of antimony-doped tin dioxide nano-slurry

A technology of tin dioxide and nano-slurry, which is applied in the direction of tin oxide, nanotechnology, nanotechnology, etc., can solve the problems of uneven dispersion, difficult dispersion, and difficult washing and removal of chloride ions, so as to avoid hard agglomeration and ensure optical performance , to avoid the effect of larger particles

Active Publication Date: 2014-03-12
FIRST NEW MATERIAL TECH DEV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the preparation of ATO powder is mainly through the solid-phase method and the liquid-phase chemical co-precipitation method using tin and antimony chloride as raw materials, but the solid-phase method has a high reaction temperature in the preparation of ATO powder, and the mixed Uneven heterogeneity, large particle size, and easy introduction of impurities; while the preparation of ATO powder by co-precipitation method has chloride ions that are extremely difficult to wash and remove. Dispersion can only be achieved through high-energy ball milling and adding a large amount of dispersant, and the dispersed particles are larger and less stable
As a result, the nano-ATO slurry made by the current preparation method has problems such as large particles, uneven dispersion, and poor stability.
However, in the current hydrothermal synthesis method, the conventional hydrothermal method adopted cannot obtain suitable Sb 3+ / Sb 5+ Ratio, and limited by the reaction pressure and temperature, it is impossible to prepare ATO slurry with good optical properties and effective absorption of near-infrared rays

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preparation example Construction

[0029] The embodiment of the present invention provides a preparation method of nano-antimony-doped tin dioxide (ATO) slurry, the method directly obtains ATO slurry by chemical reaction, without ATO powder dispersion, and the infrared absorption effect of nano-ATO slurry is good , the process is simple, the energy consumption is low, and the ATO slurry with a particle size of 20-150nm and good stability and dispersion can be prepared. The method includes:

[0030] A salt solution of tin and antimony composed of any one of tin tetrachloride, ethanol, antimony trichloride and antimony pentachloride, and a lye composed of sodium hydroxide or ammonia;

[0031] Add the alkali solution dropwise to the salt solution until the pH value of the system is adjusted to 0.8-2, add hydrogen peroxide, and part of the Sb in the system 3+ Oxidized to Sb 5+ , to obtain precipitated tin antimony hydroxide, washing and filtering the tin antimony hydroxide, adding a dispersant, stirring and dispe...

Embodiment 1

[0050] The present embodiment provides a kind of preparation method of nano antimony-doped tin dioxide (ATO) slurry, comprising:

[0051] Weigh 26g of tin tetrachloride, add it to 70ml of ethanol to form a tin tetrachloride ethanol solution, then weigh 7.6g of antimony trichloride and add it to the tin tetrachloride ethanol solution, stir at 70°C for 30 minutes to obtain a metal salt mixture (i.e. salt solution), then weigh a certain amount of 1mol / L sodium hydroxide solution (i.e. lye), add it dropwise to the metal salt mixture until the pH of the metal salt mixture is 2, add 7.5g The hydrogen peroxide with a mass concentration of 30% was continued to control the temperature at 70°C and stirred for 1 hour to obtain a suspension of tin antimony hydroxide;

[0052] The obtained tin-antimony hydroxide suspension was centrifuged at 5000rmp for 10 minutes to obtain the precipitated tin-antimony hydroxide. The obtained tin-antimony hydroxide was washed three times, and the tin-anti...

Embodiment 2

[0056] The present embodiment provides a kind of preparation method of nano antimony-doped tin dioxide (ATO) slurry, comprising:

[0057] Weigh 260g of tin tetrachloride and add it to 250ml of ethanol to form a tin tetrachloride ethanol solution, then weigh 11.4g of antimony trichloride and add it to the tin tetrachloride ethanol solution, stir at 70°C for 30 minutes to obtain a metal salt mixture solution (i.e. salt solution), then weigh a certain amount of 1mol / L sodium hydroxide solution (i.e. lye), and add it dropwise to the metal salt mixture until the pH of the metal salt mixture is 0.8, then add 11.3g The hydrogen peroxide with a mass concentration of 30% was continued to control the temperature at 70°C and stirred for 1 hour to obtain a suspension of tin antimony hydroxide;

[0058] Centrifuge the obtained tin antimony hydroxide suspension at 5000rmp for 10 minutes to obtain precipitated tin antimony hydroxide, wash the obtained tin antimony hydroxide three times, add ...

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Abstract

The invention discloses a preparation method of antimony-doped tin dioxide nano-slurry, belonging to the field of preparation of chemical raw materials. The method comprises the following steps of: preparing a saline solution of tin and antimony consisting of nitrate of tin, ethanol and nitrate of antimony, and an alkaline liquor consisting of sodium hydroxide or ammonia water; dropwise adding the alkaline liquor into a saline solution till the pH value of a system is adjusted to 0.8-2, adding hydrogen peroxide, oxidizing a part of Sb<3+> in the system into Sb<5+> to obtain a precipitated tin-antimony hydroxide, washing the tin-antimony hydroxide with water, filtering, adding a dispersing agent, and stirring and dispersing into water to obtain a tin-antimony hydroxide dispersed solution; and performing hydro-thermal treatment on the hydroxide dispersed solution in a high-pressure reaction kettle to obtain antimony-doped tin dioxide nano-slurry. The method has the advantages of simple process, low energy consumption, high dispersity of prepared slurry and stable performance.

Description

technical field [0001] The invention relates to the field of preparation of chemical raw materials, in particular to a preparation method of antimony-doped tin dioxide nano slurry. Background technique [0002] Antimony-doped tin oxide (antimony-doped tin oxide, ATO) is an important semiconductor material, which has special electrical and optical properties, such as transparent conductivity, transparent heat insulation. ATO sol is widely used in the preparation of transparent heat-insulating coatings for glass because of its ability to absorb near-infrared rays. The introduction of nanostructures is very important for improving the transparency of ATO. [0003] The main preparation methods of nano-ATO slurry reported in the existing literature include hydrothermal synthesis, ball milling dispersion, sand milling dispersion and so on. For example, (1) the Chinese invention patent application with application number 03114873.5 discloses a method for preparing ATO water-based...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02B82Y30/00B82Y40/00
Inventor 刘东华
Owner FIRST NEW MATERIAL TECH DEV