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Preparation method of doped stannic oxide conductive nano powder

A technology of conductive nano and tin dioxide, applied in the field of nano materials, can solve problems such as kettle body corrosion, corrosion equipment, danger, etc., and achieve the effect of being conducive to industrialization, simple process and good reproducibility

Active Publication Date: 2014-11-19
PANZHIHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of tin dioxide nanomaterials in this patent mainly uses SnCl 4 , SnCl 2 and other raw materials, which will introduce chloride ion impurities that are difficult to remove. The presence of chloride ions has an adverse effect on doped tin dioxide nanomaterials. For example, in fluorine-doped tin dioxide (FTO), chloride ions can be doped into the The tin oxide lattice replaces oxygen, thereby reducing the effective doping amount of fluorine element, resulting in a decrease in the conductivity of FTO
In addition, chloride ions will corrode the kettle body in a hydrothermal environment, and the corrosion of the autoclave is more dangerous to the further production.
The preparation of doped tin dioxide in these patents is complicated, and the corrosion equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Weigh 0.02mol of stannous oxalate in a 100mL beaker, add 0.06mol of 30% hydrogen peroxide in an ice-water bath, and form a transparent solution after 5 minutes of reaction; add 40mL of water to the solution and stir evenly, then add to the solution Add 0.0002mol ammonium fluoride; after fully dissolving, put the above solution in a 100mL autoclave, and place the autoclave at 180°C for 24 hours; after the reaction is completed, take out the autoclave and place it at room temperature, and the product is washed and dried. A dark green fluorine-doped tin dioxide conductive nanopowder was obtained. The powder was pressed into a disc with a diameter of 1 cm and a thickness of about 1.5 mm by a tablet press at 1.5 MPa, and the measured resistance was 38Ω / □, and □ represented the disc.

[0023] figure 1 This is the TEM image of the fluorine-doped tin dioxide conductive nanopowder prepared in Example 1. figure 1 It shows that the particle size distribution of the fluorine-dope...

Embodiment 2

[0026] Weigh 0.02mol of stannous oxalate in a 100mL beaker, add 0.08mol of 30% hydrogen peroxide in an ice-water bath, and form a transparent solution after 4 minutes of reaction; add 45mL of water to the solution and stir evenly, then add to the solution Add 0.0005mol sodium fluoride; after fully dissolving, put the above solution in a 100mL autoclave, and place the autoclave at 160°C for 48 hours; after the reaction is completed, take out the autoclave and place it at room temperature, and the product is washed and dried. A dark green fluorine-doped tin dioxide conductive nanopowder was obtained. The powder was pressed into a disc with a diameter of 1 cm and a thickness of about 1.5 mm by a tablet press at 1.5 MPa, and the measured resistance was 72Ω / □.

Embodiment 3

[0028] Weigh 0.03 mol of stannous oxalate in a 100 mL beaker, add 0.1 mol of 30% hydrogen peroxide in an ice-water bath, and form a transparent solution after 6 minutes of reaction; add 35 mL of water to the solution and stir evenly, then add to the solution Add 0.001mol antimony potassium tartrate; after fully dissolving, put the above solution in a 100mL autoclave, and place the autoclave at 200°C for 18 hours; after the reaction is completed, take out the autoclave and place it at room temperature, and the product is washed and dried. A brown antimony-doped tin dioxide conductive nanopowder is obtained. The powder was pressed into a disc with a diameter of 1 cm and a thickness of about 1.5 mm by a tablet press at 1.5 MPa, and the measured resistance was 66Ω / □.

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Abstract

The invention belongs to the field of nano materials, and particularly relates to a preparation method of doped stannic oxide conductive nano powder. The preparation method is characterized by preparing the nano powder through a hydrothermal method. The method provided by the invention comprises the following steps of weighing stannous oxalate, adding hydrogen peroxide in an ice-water bath; adding water when the above system reacts to form a transparent solution; adding a fluorine- or stibium-containing material in the solution as a dopant; mixing uniformly; carrying out hydro-thermal treatment; washing and drying to obtain the doped stannic oxide conductive nano powder. The preparation method can obtain the doped stannic oxide conductive nano powder with uniform particle size, good dispersibility and high purity without high-temperature calcination. The preparation method has easily-available raw materials, extremely simple flow, high efficiency and good repeatability, and is beneficial for large-scale production.

Description

technical field [0001] The invention belongs to the field of nanometer materials, in particular to a preparation method of tin dioxide-doped conductive nanopowder. Background technique [0002] Tin dioxide (SnO 2 ) is an n-type semiconductor material, which has the advantages of good chemical stability and optical anisotropy, and is widely used in gas-sensing materials, optoelectronic materials, lithium-ion battery materials and other fields. The conductivity of undoped tin dioxide is low, and its conductivity is greatly improved when doped with elements such as fluorine, antimony, and indium. [0003] Hydrothermal method is one of the commonly used methods for preparing doped tin dioxide nanopowders. Patent CN102491408B discloses a preparation method of antimony-doped tin dioxide nano-slurry, which mainly uses tin nitrate, ethanol, antimony nitrate, etc. as raw materials, and prepares antimony-doped tin dioxide nano-slurry through a hydrothermal process material. Patent...

Claims

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Application Information

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IPC IPC(8): C01G19/02B82Y30/00
Inventor 周才龙李玉峰
Owner PANZHIHUA UNIV
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