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Preparation method for antimony-doped tin oxide powder

A tin dioxide and antimony doping technology, which is applied in the field of nanomaterials, can solve the problems of poor powder performance and large difference in hydrolysis rate, and achieve the effect of good dispersion and fine and uniform particles

Inactive Publication Date: 2014-02-05
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But these traditional co-precipitation methods have some defects: (1) Sn 4+ , Sb 3+ The hydrolysis rate is quite different, and it is difficult to form Sn(OH) 4 , Sb(OH) 3 Co-precipitation, the final ATO nanopowder can not achieve real doping, and the performance of the obtained powder is poor

Method used

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  • Preparation method for antimony-doped tin oxide powder
  • Preparation method for antimony-doped tin oxide powder
  • Preparation method for antimony-doped tin oxide powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Dissolve 8.76g of tin tetrachloride pentahydrate, 0.57g of antimony trichloride (10% doped with antimony) and 0.32g of tartaric acid in 40mL of 2mol / L hydrochloric acid solution to obtain a transparent solution A. Dilute concentrated ammonia water with a mass fraction of 25% to 1mol / L to obtain solution B. The bottom solution is a mixture of 150mL deionized water and 150mL ethanol, and 3g polyethylene glycol-2000 is added as a dispersant, which is solution C.

[0035] (2) Add solution A and solution B dropwise to solution C in the way of double titration, the dropping time is 53min, the stirring speed is 350rpm, and the reaction temperature is controlled at 55°C.

[0036] (3) After the titration reaction is completed, control the pH of the reaction end point at 5-6, and ripen for 2 hours; obtain a light yellow precursor suspension;

[0037] (4) Suction filter the cured precursor suspension, wash with deionized water, detect chloride ions in the filtrate with silver...

Embodiment 2

[0046] (1) Dissolve 8.76g of tin tetrachloride pentahydrate, 0.86g of antimony trichloride (15% of the amount of antimony doped) and 0.40g of citric acid in 40mL of 2mol / L hydrochloric acid solution to obtain a transparent solution A. Dilute concentrated ammonia water with a mass fraction of 25% to 1mol / L to obtain solution B. The bottom solution is a mixture of 200mL deionized water and 100mL ethanol, and 1.5g polyvinyl alcohol is added as a dispersant, which is solution C.

[0047] (2) Add A and B solutions dropwise to the bottom solution C in a double titration manner, the dropping time is 65min, the stirring speed is 600rpm, and the reaction temperature is controlled at 55°C.

[0048] (3) After the titration reaction, control the pH of the reaction end point at 5-6, and ripen for 4 hours.

[0049] (4) Suction filter the cured precursor suspension, wash with deionized water, detect chloride ions in the filtrate with silver nitrate, stop washing with water until no chloride...

Embodiment 3

[0058] (1) Dissolve 10.51g of tin tetrachloride pentahydrate, 1.18g of antimony trichloride (17% doped with antimony) and 0.41g of tartaric acid in 40mL of 2mol / L hydrochloric acid solution to obtain a transparent solution A. Dilute concentrated ammonia water with a mass fraction of 25% to 1mol / L, which is solution B, and the bottom solution is a mixture of 150mL deionized water and 150mL ethanol with 0.8g CTAB added as a dispersant, which is solution C.

[0059] (2) Add solution A and solution B dropwise to bottom solution C in a double titration manner, the dropping time is 80min, the stirring speed is 800rpm, and the reaction temperature is controlled at 55°C.

[0060] (3) After the titration reaction, control the pH of the reaction end point at 5-6, and ripen for 2 hours.

[0061] (4) Suction filter the cured precursor suspension, wash with deionized water, detect chloride ions in the filtrate with silver nitrate, stop washing with water until no chloride ions are detected...

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Abstract

The invention relates to a preparation method for antimony-doped tin oxide powder. The preparation method comprises the following steps of mixing antimony trichloride, tin tetrachloride pentahydrate and a compounding ingredient, adding into a hydrochloric acid solution, and uniformly stirring a mixed solution to obtain transparent liquid; uniformly mixing a dispersing agent, tin tetrachloride pentahydrate, water and ethanol to obtain a base solution; dropwise adding the transparent liquid and an ammonium hydroxide precipitating agent into the base solution within 30 to 80 minutes in a double titration way, controlling reaction temperature to be 50 to 60 DEG C while stirring, and controlling final reaction pH to be 5 to 6; stopping stirring after titration, and performing curing to obtain precursor suspension; performing filtration, water washing, alcohol washing, azeotropic distillation, drying, grinding and calcination on obtained precursor precipitates. According to the method, tin and antimony are synchronously hydrolyzed and precipitated, and antimony is uniformly doped; the powder prepared by the method has the advantages of small particle size, loose structure, low agglomeration rate, high dispersibility and the like.

Description

technical field [0001] The invention belongs to the field of nanometer materials, and in particular relates to a preparation method of antimony-doped tin dioxide which can be used for transparent heat-insulating coatings. Background technique [0002] Antimony doped Tin Oxide (ATO) is an N-type semiconductor with stable chemical properties, low resistance, wear resistance, and corrosion resistance. It is a new multifunctional material with broad application prospects. Antistatic plastics, heat insulating coatings, fibers, anti-radiation antistatic coating materials, electrode materials, infrared absorbing heat insulating materials, sensitive components, etc. are widely used, and their preparation and application have attracted more and more attention. [0003] As a new type of energy-saving and environmentally friendly material, nano-transparent insulating glass coating has attracted great attention from academic and industrial circles. This coating incorporates spectrally ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/02C09D7/12C09D175/04
Inventor 蔡智奇韩迪文秀芳皮丕辉陆园韩太亮徐守萍程江黄宏亭蔡森
Owner SOUTH CHINA UNIV OF TECH
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