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Method for preparing antimony doped stannic oxide nano powder

A nano-powder, tin dioxide technology, applied in the field of nano-materials, can solve the problems of increased production cost, failure to achieve uniform doping of ATO nano-powder, difficulty in washing, etc.

Inactive Publication Date: 2009-12-09
NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] (1) Due to Sn 4+ and Sb 3+ The solubility product gap is large, making its hydrolysis asynchronous, and the ATO precursor prepared by the co-precipitation reaction is actually Sn(OH) 4 and Sb 4 o 5 Cl 2 Inhomogeneous mixture of the two kinds of precipitation, the ATO nanopowder finally prepared failed to achieve uniform doping in the true sense;
[0006] (2)Sn 4+ and Sb 3+ Both are easily hydrolyzed. In order to ensure that both tin and antimony exist in the form of ions, a large amount of acid must be added when preparing the mixed solution, and a large amount of alkali must be added when the precipitation reaction is carried out, which not only introduces a large amount of impurity ions, but also makes subsequent washing difficult. , also led to an increase in production costs;
[0007] (3) During the preparation of ATO nanopowders by conventional methods, due to Na + , Cl - The existence of the powder will cause the agglomeration of the powder and affect the performance of the powder;

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Take 2.96g of tin particles, 0.36g of antimony trioxide powder and 0.38g of tartaric acid and dissolve them in 320ml of 5mol / L nitric acid to prepare a light blue transparent solution; (2) Measure 100ml of deionized water into 1L of In the beaker, add 2.7g of polyethylene glycol, stir evenly, and heat in a water bath at 60°C; (3) drop the light blue transparent solution prepared in (1) and 5mol / L ammonia water into (3) ) in the bottom liquid shown in ) to control a certain titration rate for 30 minutes, then continue to stir for 30 minutes and then age for 2 hours. The reaction conditions are: the reaction temperature is 60 ° C, and the titration end point pH=3; Add 100g of deionized water to wash and centrifuge three times, then add 79g of absolute ethanol to wash with alcohol and then centrifuge three times; (5) add 121g of n-butanol to the precursor after (4) washing Azeotropic distillation; (6) drying the precursor at 60°C; (7) grinding the precursor obtained af...

Embodiment 2

[0020] (1) Add 5.4g of tin particles, 0.36g of antimony trioxide powder and 0.52g of citric acid into 320ml of 5mol / L nitric acid and dissolve to prepare a light blue transparent solution; (2) Measure 100ml of deionized water to 1L In a beaker, add 0.76g of absolute ethanol, stir evenly, and heat in a water bath at 55°C; (3) drop the light blue transparent solution prepared in (1) and 5mol / L ammonia water into (3) ) in the bottom solution shown in ) to control a certain titration rate for 30 minutes after titration, continue to stir for 30 minutes and then age for 2 hours. Add 100g of deionized water to wash and centrifuge for five times, then add 78g of isopropanol to wash with alcohol and then centrifuge for five times; (5) add 127g of n-butyl to the precursor after (4) washing Alcohol and xylene were subjected to azeotropic distillation; (6) the precursor was dried at 60°C; (7) the precursor obtained after the treatment in (6) was ground and placed in a muffle furnace for c...

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PUM

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Abstract

The invention relates to a method for preparing antimony doped stannic oxide nano powder and belongs to the field of nanometer materials. The nanometer material is prepared by the following steps that: stannum granules, antimonous oxide powder and an antimony compounding agent in a certain mixing ratio are dissolved in hydrogen nitrate at certain concentration to form light cyan transparent solution; the transparent solution and ammonia water at certain concentration are dripped into a base solution doped with a dispersing agent in a cocurrent flow mode to undergo a coprecipitation reaction; and the ATO nano powder is prepared by washing, azeotropic distillation, drying and calcining of the product of the coprecipitation reaction. The method is characterized in that: the stannum granules and the antimonous oxide powder are used as basic raw materials, the antimony compounding agent is added in a preparation process to process a precursor together with an azeotropic distillation method to prepare the ATO nano powder. The method is easy in accurate measurement, effectively suppresses the early hydrolysis of the antimony, realizes even doping of the ATO nano powder, effectively removes moisture in the precursor and free hydroxyls on the surface, reduces the conglobation of the powder, simplifies a preparation process, reduces preparation period and expends the application range of the ATO nano powder.

Description

technical field [0001] The invention belongs to the field of nanomaterials, in particular to a method for preparing antimony-doped tin dioxide nanopowder Background technique [0002] The invention is to develop a method for preparing antimony-doped tin dioxide nanometer powder. The method uses tin particles and antimony trioxide as basic raw materials, tartaric acid as a complexing agent, and ammonia water as a precipitating agent to prepare a precursor by co-precipitation, and azeotropic distillation is used to treat the precursor to prepare antimony-doped bismuth Tin oxide nanopowder. The method is simple, the process flow is short, uniform doping is realized, the prepared powder has less agglomeration, small particle size and uniform distribution, and has excellent optical and electrical properties. [0003] Antimony doped tin oxide (ATO) nanopowder combines the advantages of ATO material and nanopowder, and is a new type of functional material that has developed rapid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82B3/00
Inventor 郑占申张榜闫培起任韩娟
Owner NORTH CHINA UNIVERSITY OF SCIENCE AND TECHNOLOGY
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