Preparation method of tin antimony oxide nanopowder

A nano-powder and antimony tin oxide technology is applied in the field of preparation of tin and antimony oxide nano-powder, which can solve the problems of low purity of nano-powder, easy agglomeration between particles, wide particle size distribution, etc., and achieve excellent optical properties. and electrical properties, the elimination of hydrogen bonds, the effect of narrow distribution

Inactive Publication Date: 2016-09-07
GUANGXI NATUO TECH CO LTD
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Problems solved by technology

However, the purity of the nanopowder produced by these preparation methods is not high, the particles are easy to agglomerate, and the particle size distribution range is relatively wide.
Moreover, most processes use water as the reaction medium, resulting in obvious defects in the performance of nano-powders. On the one hand, due to factors such as the surface tension of water, there are hydrogen bonds and capillary action between the precursor particles, and a large amount of OH ˉ Adsorbed on the surface of the particles, it is easy to agglomerate between the particles; on the other hand, in order to ensure that both tin and antimony exist in the solution medium in the form of ions, a certain amount of compounding agent and dispersant must be added when preparing the mixed solution, although it can reduce sn 4+ , Sb 3+ Hydrolysis, but at the same time a large number of impurity ions are introduced, affecting product performance; or a large amount of ethanol is required to wash the precursor to remove chloride ions, which indirectly greatly increases the production cost

Method used

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  • Preparation method of tin antimony oxide nanopowder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] 13.84g SnCl 4 And 3.13g SbCl 3 Dissolve in 65mL of anhydrous ethanol solution to obtain a colorless and transparent tin-antimony mixed solution. Mix 7.0g of ammonium bicarbonate with 70.0g of anhydrous ethanol solution to make a slurry, then dissolve 0.1g of ammonium acetate in a small amount of ethanol and add it to the dispersion, A solid-liquid suspension mixed solution is obtained. Under stirring conditions, the tin-antimony solution and the solid-liquid suspension were mixed and reacted. The reaction temperature was 5°C, the pH value was 5, and the reaction time was 2.0h to obtain white milky Sn(OH) 4 And NH 4 The Cl mixture precipitated. After filtration and vacuum drying at 40°C, after recovering the ethanol, the filter cake was dissolved and dispersed with 70.0g deionized water, filtered, washed with deionized water until no chloride ions were detected, and then dehydrated with absolute ethanol. Vacuum drying at 90℃ to obtain white powdery Sn(OH) 4 The precursor ...

Embodiment 2

[0029] 10.70g SnCl 4 And 2.35g SbCl 3 Dissolve in 35mL of anhydrous ethanol solution to obtain a colorless and transparent tin-antimony mixed solution. Mix 9.0g of ammonium bicarbonate with 50.0g of anhydrous ethanol solution to make a slurry, and then dissolve 0.6g of ammonium acetate in a small amount of ethanol and add to it, disperse, A solid-liquid suspension mixed solution is obtained. Under stirring conditions, the tin-antimony solution and the solid-liquid suspension were mixed and reacted. The reaction temperature was 15°C, the pH value was 6, and the reaction time was 3.5 hours to obtain white milky Sn(OH) 4 And NH 4 The Cl mixture precipitated. After filtering, drying in vacuum at 60°C, and recovering ethanol, the filter cake is dissolved and dispersed with 110.0g deionized water, filtered, washed with deionized water until no chlorine ions are detected, and then dehydrated with absolute ethanol. Vacuum drying at 80℃ to obtain white powdery Sn(OH) 4 The precursor was...

Embodiment 3

[0032] 16.43g SnCl 4 And 0.78g SbCl 3 Dissolve in 65mL of anhydrous ethanol solution to obtain a colorless and transparent tin-antimony mixed solution. Mix 14.0g of ammonium bicarbonate with 35.0g of anhydrous ethanol solution to make a slurry, then dissolve 0.6g of ammonium acetate in a small amount of ethanol and add to it to disperse. A solid-liquid suspension mixed solution is obtained. Under stirring conditions, the tin-antimony solution and the solid-liquid suspension were mixed and reacted. The reaction temperature was 25°C, the pH value was 8, and the reaction time was 4.0 hours to obtain white milky Sn(OH) 4 And NH 4 The Cl mixture precipitated. After filtration and vacuum drying at 70°C, after recovering ethanol, the filter cake was dissolved and dispersed with 90.0g deionized water, filtered and washed with deionized water until no chloride ions were detected, and then dehydrated with absolute ethanol. Vacuum drying at 60℃ to obtain white powdery Sn(OH) 4 The precurs...

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Abstract

The invention discloses a preparation method of tin antimony oxide (ATO) nano powder. The preparation method comprises the following steps: by adopting antimony salt and tin salt as reaction raw materials, adopting ammonium hydrogen carbonate as a neutralization agent, adopting ammonium acetate as a cosolvent and adopting high-concentration ethanol as a reaction medium, performing solid-liquid heterophase coprecipitation reaction to generate Sn(OH)4 and NH4Cl mixed precipitates, performing filtration and vacuum drying, and then dissolving and dispersing a filter cake by using deionized water, then filtering, washing, dehydrating, drying, calcining and crushing to obtain the ATO nano powder. The preparation method disclosed by the invention is safe and environment-friendly, and is simple in process and low in cost; and an ATO nano powder product prepared by using the method disclosed by the invention is less in aggregate, uniform in doping, small in particle size and narrow in distribution range, and has excellent optical and electrical properties.

Description

Technical field [0001] The invention belongs to the field of tin oxide antimony nano powder, and particularly relates to a preparation method of tin antimony nano powder. Background technique [0002] Energy saving and environmental protection have become a topic of global concern today, and energy-saving, environmentally friendly, high-tech products and materials are gradually being favored by people. Nano antimony tin oxide (ATO) is an n-type semiconductor material with a wide energy gap, with optical and physical properties that macro-sized objects do not have. It exhibits high absorptivity, transmittance and reflectivity in the ultraviolet, visible and near-infrared regions in turn. It can be added to various coatings to make transparent, heat-insulating and anti-static multifunctional This type of material is widely used in energy conservation and environmental protection fields such as construction, electronic communication and catalysis. [0003] The preparation of nano an...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G30/00C01G19/02B82Y30/00
CPCB82Y30/00C01G30/00C01P2004/04C01P2004/64C01P2006/10C01P2006/12C01P2006/40
Inventor 尹作栋刘炳山孙皓刘旭
Owner GUANGXI NATUO TECH CO LTD
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