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A kind of method for preparing tin dioxide nanopowder rich in oxygen vacancies and products therefrom

A technology of tin dioxide and nanopowder, applied in the direction of tin oxide, nanotechnology for materials and surface science, nanotechnology, etc., can solve the safety risk of reducing gas and the increase in cost, increase in cost, increase in production process, etc. problems, to achieve the effect of reducing the secondary heat treatment process, less pollution, and good dispersion

Inactive Publication Date: 2017-06-23
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this type of method, on the one hand, the use of reducing gas will bring safety risks and cost increases; on the other hand, it is necessary to prepare tin dioxide nanopowder first and then perform secondary heat treatment on it, which increases the production process and causes costs. rise

Method used

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  • A kind of method for preparing tin dioxide nanopowder rich in oxygen vacancies and products therefrom
  • A kind of method for preparing tin dioxide nanopowder rich in oxygen vacancies and products therefrom
  • A kind of method for preparing tin dioxide nanopowder rich in oxygen vacancies and products therefrom

Examples

Experimental program
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Effect test

Embodiment 1

[0027] with SnCl 4 ·5H 2 O is a tin salt, and NaOH is a precipitating agent:

[0028] (1) The preparation concentration is 0.5 mol L -1 SnCl 4 aqueous solution, add 1.0 mol L to it while stirring -1 NaOH aqueous solution, make the pH value of the uniform white precipitate suspension system obtained after mixing be 7.0, continue to stir for 20 min;

[0029] (2) Centrifuge the white precipitate suspension described in step (1), wash the precipitate with water for 3 times, and then dry at 80°C to obtain tin dioxide precursor powder;

[0030] (3) The tin dioxide precursor powder obtained in step (2) was subjected to vacuum heat treatment, the vacuum degree was set to 0.05 Pa, the heating rate was 5 °C / min, the temperature was kept at 500 °C for 1.5 h, and the product was obtained after natural cooling.

[0031] The powder X-ray diffraction (XRD) pattern and optical digital photos of the product are shown as figure 1 (a) and (b) shown. It can be seen from the figure that th...

Embodiment 2

[0033] The tin source, technological process, and technological parameters used in Example 1 are the same, except that KOH is used as the precipitating agent. The XRD figure, optical digital photo, TEM photo, HRTEM photo, ultraviolet-visible diffuse reflectance spectrum, the XPS of O1s of gained tin dioxide nanopowder are respectively compared with figure 1 (a), figure 1 (b), figure 2 (a), figure 2 (b), image 3 (a), Figure 4 (a) Approximate.

Embodiment 3

[0035] Same as Example 1, except that the heat treatment of the tin dioxide precursor powder is changed from being carried out in a vacuum environment to being carried out in air.

[0036] The XRD pattern and optical digital photo of the product are as follows Figure 5 (a) and (b) shown. It can be seen from the figure that the product obtained by heat-treating the precursor powder in air is also rutile tin dioxide, and the color is light yellow; the TEM photos and HRTEM photos of the products are as follows Figure 6 As shown in (a) and (b), it can be seen from the figure that the grain size of the tin dioxide nanopowder is about 9 nm, and the dispersion is not as good as that of the product obtained in Example 1. The HRTEM photo shows that the grain crystallinity is very good; The UV-Vis diffuse reflectance spectrum of the product is as image 3 (b), with image 3 (a) It can be seen that the tin dioxide nano-powder obtained by heat-treating the precursor powder in air has...

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Abstract

The invention discloses a preparation method of oxygen-vacancy-rich tin dioxide nanometer powder and an obtained product. The preparation method comprises the steps that an inorganic tin brine solution with the concentration of 0.2-3.0 mol L-1 is prepared, 0.5-5.0 mol L-1 of a NaOH or KOH aqueous solution is added into the inorganic tin brine solution while stirring, the pH value of a uniform white precipitate suspension system obtained after mixing is completed is regulated to 6.0-8.5, and the stirring continues for 10-60 minutes; the white precipitate suspension is subjected to solid-liquid separation, and the precipitate is washed with water for 2-5 times and then is dried at the temperature of 40-120 DEG C to obtain tin dioxide precursor powder; the tin dioxide precursor powder is subjected to vacuum heat treatment in the environment with the vacuum degree of 0.01 Pa-25 kPa, and natural cooling is performed to obtain the product, wherein the temperature rise speed is 2-15 DEG C / min, the heat preservation temperature is 250-600 DEG C, and the holding time is 0.5-4.0 hours. The preparation method utilizes a vacuum sintering process to conduct heat treatment on the tin dioxide precursor powder without secondary treatment or modification, the oxygen-vacancy-rich tin dioxide nanometer powder can be directly obtained, and the preparation method has the advantages of being simple in process, low in equipment demand, low in cost, less in pollution, suitable for mass production and the like.

Description

technical field [0001] The invention relates to a method for preparing tin dioxide nanopowder rich in oxygen vacancies and the resulting product, in particular to a method for preparing tin dioxide nanopowder rich in oxygen vacancies by vacuum heat-treating tin dioxide precursor powder, belonging to Micro-nano functional material synthesis technology field. The tin dioxide nanopowder rich in oxygen vacancies can be used in the fields of gas sensing, photocatalysis, photoelectrocatalysis, photodegradation of organic matter and the like. Background technique [0002] As a semiconductor oxide with a wide bandgap, tin dioxide has important applications in the fields of gas sensing, photocatalysis, photoelectrocatalysis, and photodegradation of organic pollutants due to its stable properties, low cost, and non-toxicity. However, in practical applications, due to the wide band gap of tin dioxide, it can only absorb ultraviolet light but not visible light, so it cannot make full u...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02B82Y30/00
CPCB82Y30/00C01G19/02C01P2002/72C01P2002/84C01P2002/85C01P2004/04C01P2004/64
Inventor 陈长龙魏玉玲
Owner UNIV OF JINAN