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Preparation method of particle size controllable tin dioxide nano-powder

A nano-powder, tin dioxide technology, applied in tin oxide and other directions, to achieve the effects of short reaction period, low cost, and easy control of the reaction process

Active Publication Date: 2017-06-20
DALIAN JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the prior art, it has always been a technical difficulty to control the particle size of tin oxide nanopowders without calcination temperature or heat treatment time. The root cause is that the growth of grains needs to be promoted by increasing temperature and time, but The growth of ultra-fine tin oxide grains and the high specific surface energy of nanoparticles will inevitably lead to the agglomeration of particles (Guo Guangsheng et al., China Powder Technology, 2003, 9: 22-24)

Method used

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Experimental program
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Effect test

Embodiment 1

[0029] Take 2.37g (0.02mol) of metal Sn grains, add it into a three-necked flask, and add 3.75ml of HNO2 dropwise to the flask 3 And 5ml HCl, and the deionized water of 8.75ml, the control reaction temperature is 80 ℃, and the reaction time is 2.5h, obtains the Sn ion solution, adds the ethanol solution of 3.53ml (equivalent to 0.2L / L) in the Sn ion solution, After adding, let stand for 12h. The above mixed solution and ammonia (25wt.%) solution were simultaneously titrated into 0.3wt.% PVA aqueous solution, the reaction temperature was controlled to be 65° C., the reaction time was 1 h, and the pH value was 3 to obtain a suspension. The suspension was left to stand for 12 hours, then filtered, washed three times with deionized water and absolute ethanol, then dried at 100°C for 5 hours, then ground and calcined at 600°C for 2 hours to obtain the final Tin oxide nanopowder.

Embodiment 2

[0031] Take 2.37g (0.02mol) of metal Sn grains, add it into a three-necked flask, and add 3.75ml of HNO2 dropwise to the flask 3 And 5ml HCl, and the deionized water of 8.75ml, control reaction temperature to be 80 ℃, reaction time is 2.5h, obtain Sn ion solution, add the HNO of 1.875ml (equivalent to 0.107L / L) in Sn ion solution 3solution, add 5.29ml (equivalent to 0.3L / L) ethanol solution to the Sn ion solution, and let stand for 12h after adding. The above mixed solution and ammonia (25wt.%) solution were simultaneously titrated into 0.3wt.% PVA aqueous solution, the reaction temperature was controlled to be 65° C., the reaction time was 1 h, and the pH value was 3 to obtain a suspension. The suspension was left to stand for 12 hours, then filtered, washed three times with deionized water and absolute ethanol, then dried at 100°C for 5 hours, then ground and calcined at 600°C for 2 hours to obtain the final Tin oxide nanopowder.

Embodiment 3

[0033] Take 2.37g (0.02mol) of metal Sn grains, add it into a three-necked flask, and add 3.75ml of HNO2 dropwise to the flask 3 And 5ml HCl, and the deionized water of 8.75ml, control reaction temperature to be 80 ℃, reaction time is 2.5h, obtain Sn ion solution, add the HNO of 3.75ml (equivalent to 0.215L / L) in Sn ion solution 3 solution, add 7.056ml (equivalent to 0.4L / L) ethanol solution to the Sn ion solution, and let stand for 12h after adding. The above mixed solution and ammonia (25wt.%) solution were simultaneously titrated into 0.3wt.% PVA aqueous solution, the reaction temperature was controlled to be 65° C., the reaction time was 1 h, and the pH value was 3 to obtain a suspension. The suspension was left to stand for 12 hours, then filtered, washed three times with deionized water and absolute ethanol, then dried at 100°C for 5 hours, then ground and calcined at 600°C for 2 hours to obtain the final Tin oxide nanopowder.

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Abstract

The invention discloses a preparation method of a particle size controllable tin dioxide nano-powder, and in particular relates to a preparation method of a high dispersibility and high crystallinity tin oxide nano-powder with a particle size of 10-18nm, i.e. ethyl nitrate assisted precipitation method. The method utilizes the auxiliary effect of ethyl nitrate formed by nitric acid and ethanol and precipitation technique to prepare tin oxide nano-powder. The tin oxide nano-powder prepared by the method has adjustable particle size, uniform particle size distribution, and good dispersion and crystallization properties, also has no need for changing the calcination temperature and heat treatment time, and has the advantages of simple process, low cost, and short preparation cycle, etc.

Description

technical field [0001] The invention relates to a preparation method of tin dioxide, in particular to a preparation method of tin dioxide nanopowder whose particle size is in the range of 10-18nm and whose particle size is controllable. Background technique [0002] Tin oxide is a wide bandgap semiconductor with a forbidden band width of 3.60eV and a bulk exciton radius of about 1.7nm. Nano-tin oxide has unique optical, electrical and catalytic properties, and is widely used in batteries, semiconductors, gas sensors and catalytic materials. In the field of catalysis, it can be used to form composite catalysts with other metals, which can be used for hydrocarbon oxidation, methanol reforming, reduction of nitrogen oxides, etc., and is also widely used in photocatalysis and electrocatalysis. These properties have a strong dependence on their specific surface, and nanoparticles with sufficiently small particle size and large specific surface area will exhibit unique properties...

Claims

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Application Information

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IPC IPC(8): C01G19/02
CPCC01G19/02C01P2002/60C01P2002/72C01P2004/04C01P2004/32C01P2004/51C01P2004/64
Inventor 刘世民梁冬冬赵东杨
Owner DALIAN JIAOTONG UNIVERSITY
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