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Method for directly synthesizing liquid phase of tin oxide nano powder

A technology of nano-powder and synthesis method, applied in the field of nano-materials, can solve the problems of chloride ion corrosion, wide particle size distribution, low powder purity, etc. The effect of narrow particle size distribution

Inactive Publication Date: 2011-05-11
DALIAN JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] There are some shortcomings in the above-mentioned methods, such as the difficulty in washing chlorine ions with chlorine salt as raw material, the chlorine ions remaining in the powder will corrode the device and hinder the densification of the target material; if the sol-gel The glue method or the reverse micellar method has problems such as serious waste of organic matter, high cost and serious agglomeration; if the hydrothermal or alcohol thermal method is used, there are difficulties such as expensive equipment, low output, and difficult industrial production; if the mechanical method is used, the powder purity is low , wide particle size distribution and other defects; other methods also use organic reagents, need a large amount of lye to neutralize, and require a large amount of ethanol to wash, etc.

Method used

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  • Method for directly synthesizing liquid phase of tin oxide nano powder
  • Method for directly synthesizing liquid phase of tin oxide nano powder
  • Method for directly synthesizing liquid phase of tin oxide nano powder

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Weigh 5g of metal tin particles, measure 30ml of 7.5mol / L nitric acid, and 0.15g of polyvinyl alcohol, mix metal tin and nitric acid and stir at 95 degrees Celsius for 2.5 hours to obtain a white colloidal precipitation precursor, and let the body stand Filter after 24 hours. The filtrate obtained by filtration contains nitric acid and is recovered for reuse. The filter cake is rinsed with deionized water for 5 times and then placed in a drying oven for 5 hours at 100 degrees Celsius. After the dried precursor is cooled to room temperature, it is ground and dried for 200 Mesh sieve. Finally, the precursor obtained by sieving was calcined at 350 degrees Celsius for 2 hours to obtain light yellow-green tin oxide nanopowder. figure 1 The X-ray diffraction pattern of the powder obtained by calcination at 350 degrees Celsius. The results show that the powder is tin oxide with tetragonal rutile structure, and there are no other impurities in the powder. figure 2 A is the ...

Embodiment 2

[0031] Weigh 3 g of metal tin particles, measure 20 ml of 7.5 mol / L nitric acid, mix metal tin and nitric acid and stir at 82 degrees Celsius for 2 hours to obtain a white colloidal precipitate precursor, which is left to stand for 15 hours and then filtered. The filtrate obtained by filtration contains nitric acid and is recovered for reuse. The filter cake is rinsed with deionized water for 3 times and then placed in a drying oven for 5 hours at 100 degrees Celsius. After the dried precursor is cooled to room temperature, it is ground and dried for 200 Mesh sieve. Finally, the precursor obtained by sieving was calcined at 350 and 550 degrees Celsius for 2 hours respectively to obtain light yellow-green tin oxide nanopowder. figure 2 B and figure 2 C are TEM micrographs of powders calcined at 350 and 550 degrees Celsius, respectively. The results show that the particle size of the tin oxide powder obtained at 350h and 550 degrees Celsius is within 10-30nm, and the shape i...

Embodiment 3

[0033] Weigh 5g of metal tin particles, measure 30ml of 7.5mol / L nitric acid, and 0.05g of polyvinyl alcohol, mix metal tin and nitric acid, and stir at 65 degrees Celsius for 2.5 hours to obtain a white colloidal precipitation precursor. Filter after 6 hours. The filtrate obtained by filtration contains nitric acid and is recovered for reuse. The filter cake is rinsed with deionized water for 3 times and then placed in a drying oven for 3 hours at 80 degrees Celsius. After the dried precursor is cooled to room temperature, it is ground and dried for 200 Mesh sieve. Finally, the precursor obtained by sieving is calcined at 600 degrees centigrade for 1 hour to obtain a spherical light yellow-green tin oxide nanopowder with a particle size of 15-25 nm.

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Abstract

The invention relates to a method for directly synthesizing liquid phase of tin oxide nano powder, which comprises the following steps of: mixing metallic tin particles with nitric acid and polyvinyl alcohol of certain concentrations in a certain mol ratio; synthesizing a white colloid-like precipitation precursor at a certain reaction temperature while stirring; standing the precursor for a certain period of time, and then filtering and reclaiming the nitric acid for reuse; and leaching the precipitate by deionized water, drying the precipitate at a temperature of between 50 and 150 DEG C for 0.5 to 5 hours, grinding the precipitate, and calcining the precipitate at a temperature of between 300 and 900 DEG C for 0.5 to 4 hours to obtain the undertint yellow-green tin oxide nano powder. The tin oxide nano powder obtained by the method has high powder purity, good dispersity and fewer agglomerations, the grain diameter is between 5 and 30 nm, the distribution range of the grain diameter is narrow, and the shape of the tin oxide nano powder is spherical or quasi-spherical.

Description

technical field [0001] The invention relates to the field of nanometer materials, in particular to a method for preparing a tin oxide nanometer material with gas-sensing performance and photoelectric performance. Background technique [0002] Tin oxide is an important gas-sensing material, transparent conductive electrode material, catalyst and catalyst carrier material. In recent years, the preparation of tin oxide nanopowders has attracted more and more attention. This is mainly because the smaller the particle size of the powder, the larger the specific surface area of ​​the powder, so that the performance of the device prepared by using the powder is better. For example, the sensitivity of gas sensors increases with the decrease of tin oxide powder particle size; the catalytic performance of tin oxide as a catalyst also increases with the decrease of powder particle size; When the target is sintered with tin oxide, the sintering temperature of the target can be reduced...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02B82B3/00
Inventor 柴卫平刘世民
Owner DALIAN JIAOTONG UNIVERSITY