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Method for preparing stibium doped stannic oxide nano-powder

A technology of antimony-doped tin oxide and nanopowder, which is applied in tin oxide, nanotechnology, nanotechnology, etc., can solve the problems of high powder resistance, uneven dopant dispersion, and large particle size impurities, and achieve excellent electrical resistance. properties, uniform dopant distribution, and small particle size effects

Inactive Publication Date: 2013-03-20
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The sol-gel method uses metal alkoxides as raw materials, so the cost is relatively high, and it is difficult to realize industrialization
Chinese patent CN200710020429.7 discloses a preparation method named as , which uses a combustion method to prepare antimony-doped tin oxide nanocrystals, but the synthesis temperature is high, the powder is not uniformly doped, the particle size is large, and impurities are easily introduced. The powder has high resistance and cannot meet the requirements of use, so it is rarely used in the synthesis of ATO nanopowders
Chinese patent CN200810126171.3 discloses a preparation method of antimony-doped tin oxide material. The patent uses chemical co-precipitation method, but the current chemical co-precipitation method is not suitable for preparing high-performance nano-ATO powder, mainly because Sb 3+ and Sn 4 with OH - The solubility products differ greatly (respectively 4.0*10 -42 and 1.0*10 -56 ), when NaOH and other alkalis are used as precipitants, the precipitation of Sb and Sn is not synchronized, antimony hydroxide will precipitate before tin oxide, resulting in uneven dispersion of dopants, and the final ATO powder can not achieve uniform doping in the true sense. It is not a co-precipitation in the true sense. At the same time, high-temperature calcination will increase the segregation of the two substances and seriously affect its performance.

Method used

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  • Method for preparing stibium doped stannic oxide nano-powder
  • Method for preparing stibium doped stannic oxide nano-powder
  • Method for preparing stibium doped stannic oxide nano-powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Weigh 3.506g SnC1 4 ·5H 2 O and 0.114g SbC1 3 (The molar ratio of Sb and Sn is 5:100), 50mL of absolute ethanol was added to a round bottom flask, 1ml of polyethylene glycol 400 was added, agate beads of a certain proportion were added, and ultrasonic waves were used for five minutes to make Mix evenly to obtain a mixed solution;

[0020] (2) Fix the round bottom flask on the rotary reactor, control the rotation speed at 15rad / min, and the temperature at 30°C. After stabilization, turn on the ammonia gas generator, control the flow rate of ammonia gas at 5ml / min, and transport the ammonia gas to the mixing tank through the pipeline. At the solution interface, after 1.5 hours, the mixed solution began to have a colorless, transparent, and white turbid emulsion. After continuing to react for 1 hour, stop filling the ammonia gas. After 10 minutes, increase the reaction temperature to 50°C and continue the reaction for 5 minutes, and fill the other interface with air...

Embodiment 2

[0024] Weigh 3.506g SnC1 4 ·5H 2 O and 0.114g SbC1 3 (The molar ratio of Sb and Sn is 5:100), add in 50mL absolute ethanol, weigh 1ml polyethylene glycol 400 again, disperse 5min under ultrasonic condition, make it mix uniformly, obtain mixed solution; Steps (2) and (3) of 1 obtained a white powder; the resulting white powder was calcined at 600 °C for 2 h to obtain light blue nano-Sb doped SnO 2 Particles, labeled 5%Sb-SnO 2 -600°C.

Embodiment 3

[0026] (1) Weigh 3.506g SnC1 4 ·5H 2 O and 0.228g SbC1 3 (The molar ratio of Sb and Sn is 10:100), 50 mL of absolute ethanol is added in a round-bottomed flask, 2ml of polyethylene glycol 400 is added, agate beads of a certain size are added, and the ultrasonic wave is ultrasonicated for five minutes, to disperse evenly;

[0027] (2) Fix the round-bottom flask on the rotary reactor, control the rotation speed to 30rad / min, and the temperature to 30°C. After stabilization, turn on the ammonia gas generator, control the flow rate of ammonia gas to 10ml / min, and transport the ammonia gas to the solution through the pipeline Interface, after 1.5 hours, the mixed solution began to have a colorless, transparent and white turbid emulsion. After continuing the reaction for 1 hour, stop filling the ammonia gas, stop the reaction after 10 minutes, raise the reaction temperature to 50°C for 5 minutes, and fill the other interface with air. Purify the ammonia in the device;

[0028] (...

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Abstract

The invention relates to a method for preparing a nano-material, in particular to a method for preparing stibium doped stannic oxide nano-powder. The method comprises the following steps of: dissolving SbC13 and SnC14.5H2O in absolute ethyl alcohol, adding in a dispersant, putting the obtained mixed solution in a rotating reactor, adding in a grinding auxiliary medium, conveying ammonia to the interface of the mixed solution, and reacting so as to obtain the precursor of the stibium doped stannic oxide nano-powder; filtering, alcohol washing and drying, and calcining, thereby obtaining conductive stibium doped stannic oxide powder. The method adopts the technical scheme of adding the grinding auxiliary medium under the gas-liquid reaction interface and the rotation condition; the nano-powder prepared is small in grain size and even in doping agent distribution and shows excellent electrical performance; and the resistivity of the nano-stannic oxide is reduced to 65.4 ohm.cm and the electric conductivity thereof is 0.0225 S.CM<-1>. Besides, the preparation method is simple in process and controllable in conditions, and has bright industrial popularization and application prospect.

Description

technical field [0001] The invention relates to a preparation method of nanomaterials, in particular to a preparation method of antimony-doped tin oxide nanopowder. Background technique [0002] SnO 2 It is a wide bandgap semiconductor material. When O vacancies are generated or F, Sb and other elements are doped, an N-type semiconductor is formed. It has special optical and electrical properties and has been widely studied. Among them, antimony doped tin oxide (Antimony doped tin oxide ATO), as a metal oxide with excellent electrical conductivity, has attracted more attention due to its strong mechanical properties and high thermal stability. The introduction of nanotechnology can significantly improve the performance of transparent conductive oxide materials. Nano-ATO powders are widely used in antistatic plastics, fibers, coatings, "three-proof" coating materials for displays, infrared absorption and heat insulation materials, and gas sensors. , electrochromic, solar el...

Claims

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Application Information

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IPC IPC(8): C01G19/02B82Y30/00
Inventor 王作山郑敏文彪
Owner SUZHOU UNIV
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