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Preparation method of nanoscale stannic oxide hollow sphere

A nano-tin dioxide and tin dioxide technology, applied in the field of nanomaterials, can solve the problems of adding an appropriate amount of ethylene glycol or polyethylene glycol, cracking, unevenness, etc., and achieve mild reaction conditions, regular morphology, and uniform size. Effect

Inactive Publication Date: 2012-07-18
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent whose publication number is CN 101012067A uses natural polymer powder as a sacrificial template to prepare nanoscale tin dioxide hollow sphere materials, and the Chinese patent whose publication number is CN1789140A uses zinc oxide as a sacrificial template to prepare nanoscale tin dioxide hollow sphere materials. The disadvantages of the two methods: 1) The process of removing the sacrificial template can easily cause the collapse, rupture and unevenness of the nanosphere shell; 2) The preparation process is complicated, the cost is high, and industrial production is difficult
The Chinese patent whose publication number is CN101638247A adopts the hydrothermal method to treat the stannous sulfate aqueous solution to prepare nano-scale tin dioxide hollow spheres. The experiment finds that its shortcoming is that when the concentration of stannous sulfate exceeds a certain amount, the prepared stannous oxide will be and tin dioxide, it is difficult to obtain high-purity tin dioxide
The Chinese patent with the publication number CN102086044A adopts the reaction of tin salt and alkali to prepare nanoscale tin dioxide hollow spheres. The disadvantage is that an appropriate amount of ethylene glycol or polyethylene glycol needs to be added to the precursor solution during the preparation process.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A method for preparing nano-scale tin dioxide hollow spheres uses stannous sulfate and hydrogen peroxide as reaction raw materials and is prepared by a hydrothermal method. The specific steps are as follows:

[0020] (1) Under stirring conditions, evenly disperse 2mmol of stannous sulfate in 10mL of distilled water to obtain a stannous sulfate solution A with a concentration of 200mmol / L;

[0021] (2) Under stirring conditions, add 30% hydrogen peroxide dropwise to solution A, control the molar ratio of hydrogen peroxide to stannous sulfate to 50, and adjust the pH of the solution to 2.0 with dilute sulfuric acid to obtain solution B;

[0022] (3) Transfer solution B into a 30mL stainless steel reactor lined with polytetrafluoroethylene, react at 180°C for 15 hours, cool to room temperature naturally, and obtain solid product C after separation;

[0023] (4) Repeatedly washing C with deionized water to no soluble ions to obtain a solid product D;

[0024] (5) Dry the solid produc...

Embodiment 2

[0026] A method for preparing nano-scale tin dioxide hollow spheres uses stannous oxalate and hypochlorous acid as reaction raw materials and is prepared by a hydrothermal method. The specific steps are as follows:

[0027] (1) Under stirring conditions, uniformly disperse 0.1 mmol of stannous oxalate in 10 mL of distilled water to obtain a stannous oxalate solution A with a content of 10 mmol / L;

[0028] (2) Under stirring conditions, add a 0.05M hypochlorous acid solution dropwise to solution A, control the molar ratio of hypochlorous acid to stannous oxalate to 5, and adjust the pH of the solution to 1.0 with sodium hydroxide to obtain solution B ;

[0029] (3) Transfer solution B into a 30mL stainless steel reactor lined with polytetrafluoroethylene, react at 120°C for 30 hours, cool to room temperature naturally, and obtain solid product C after separation;

[0030] (4) Repeatedly washing C with deionized water to no soluble ions to obtain a solid product D;

[0031] (5) Dry the s...

Embodiment 3

[0033] A method for preparing nano-scale tin dioxide hollow spheres uses stannous chloride and sodium hypochlorite as reaction raw materials and is prepared by a hydrothermal method. The specific steps are as follows:

[0034] (1) Under stirring conditions, disperse 5mmol of stannous chloride uniformly in 10mL of distilled water to obtain a stannous chloride solution A with a concentration of 500mmol / L;

[0035] (2) Under stirring conditions, add dropwise an aqueous solution of sodium hypochlorite with a concentration of 5M to solution A, control the molar ratio of sodium hypochlorite to stannous chloride to 10, and then adjust the pH of the solution to 4.0 with dilute hydrochloric acid to obtain a solution B;

[0036] (3) Transfer solution B into a 30mL stainless steel reactor lined with polytetrafluoroethylene, react at 230°C for 5 hours, cool to room temperature naturally, and obtain solid product C after separation;

[0037] (4) Wash C repeatedly with deionized water until there i...

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PUM

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Abstract

The invention belongs to the field of nano materials and relates to a preparation method of a nanoscale stannic oxide hollow sphere. The method is characterized in that stannous salts and oxidants serve as reaction materials and a hydro-thermal method is used for preparation under the acidic condition at the PH value between 1.0 and 4.0; the stannous salts consist of at least one of stannous sulfate, stannous chloride and stannous oxalate; the oxidants consist of at least one of hydrogen peroxide, chloric acid, hypochlorous acid, potassium chlorate, sodium chlorate, potassium hypochlorite and sodium hypochlorite; and PH value of solutions is adjusted by one of sulphuric acid, hydrochloric acid, oxalic acid and sodium hydroxide. The preparation method does not use any sacrificial templates and organic solvents and is environmentally friendly, simple in process, mild in reaction condition, low in energy consumption, easy to control, high in product purity, and suitable for large-scale industrial production. The nanoscale stannic oxide hollow sphere can be applicable to gas sensors, lithium ion batteries, catalysts and photoelectronic devices.

Description

Technical field [0001] The invention belongs to the field of nano materials, and specifically relates to a method for preparing nano-level tin dioxide hollow spheres. Background technique [0002] Tin dioxide is an important n-type wide band gap semiconductor material with a band gap width of 3.6 eV. It has broad application prospects in the fields of gas sensors, lithium ion batteries, catalysts, and optoelectronic devices. Tin dioxide with nano-scale hollow sphere structure has the characteristics of low density, high specific surface area, good permeability, etc., which greatly improves the gas sensitivity, electrochemical activity and catalytic activity of tin dioxide, which has attracted widespread attention. . [0003] Tin dioxide with nano-scale hollow sphere structure can be prepared by sacrificial template method and template-free method. The sacrificial template method uses silica balls, polymer colloidal particles or micelles formed by surfactants as the starting templa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B19/02B82Y40/00
Inventor 马希骋管从胜
Owner SHANDONG UNIV
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