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Preparation method of nanometer antimony doped tin oxide material and its high-solid-content dispersion

A technology of antimony-doped tin oxide and high solid content is applied in the field of preparation of nano-oxide materials, which can solve the problem of asynchronous hydrolysis of ions, and achieve the effect of high solid content and avoiding agglomeration.

Inactive Publication Date: 2014-09-10
SHANGHAI NAXU IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The present invention simplifies the double hydrolysis process into a single hydrolysis process to solve the problem of Sb 3+ and Sn 4+ The problem of unsynchronized ion hydrolysis, the present invention proposes nano antimony doped tin oxide material and its preparation method of high solid content dispersion liquid

Method used

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  • Preparation method of nanometer antimony doped tin oxide material and its high-solid-content dispersion
  • Preparation method of nanometer antimony doped tin oxide material and its high-solid-content dispersion
  • Preparation method of nanometer antimony doped tin oxide material and its high-solid-content dispersion

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Embodiment 1

[0021] Add 2mL of surfactant OP9 to 100mL of ethanol, stir for 20min to form a uniform mixed micellar dispersion system; then weigh 5.1583g of SbCl 3 and 2.7337g of Sb(CO 3 ) 2 Add to the above micellar dispersion system, add 0.2mL of hydrolysis inhibitor nitric acid, make SbCl 3 Slowly hydrolyzed, finally in Sb(CO 3 ) 2 A thin layer of amorphous antimony oxide hydrate Sb is uniformly formed on the surface of 2 o 3 ×xH 2 O: The precursor was calcined at 700°C for 5 hours in an air atmosphere to form an ATO powder with a primary particle size of 7-15 nm and a secondary particle size of less than 100 nm. The TEM image of the synthesized nano-scale ATO powder is as follows figure 1 shown.

Embodiment 2

[0023] In 100mL, ethanol adds the surfactant sodium cetyl sulfate of 2mL, stirs 20min to form the uniform mixed micelle dispersion system; Then weigh 9.5863g of (C 6 h 5 ) 3 SbCl 2 and 2.7337g of Sb(CO 3 ) 2 Add to the above-mentioned micelle dispersion system, add the nitric acid of hydrolysis inhibitor 0.2mL, make (C 6 h 5 ) 3 SbCl 2 Slowly hydrolyzed, finally in Sb(CO 3 ) 2 A thin layer of amorphous antimony oxide hydrate Sb is uniformly formed on the surface of 2 o 3 ×xH 2 O: The precursor was calcined at 600°C for 5 hours in an air atmosphere to form an ATO powder with a primary particle size of 7-15 nm and a secondary particle size of less than 100 nm. The SEM of the synthesized nanoscale ATO powder is as figure 2 shown.

Embodiment 3

[0025] Add 2mL of surfactant OP9 to ethanol in 100mL, stir 20min to form a uniform mixed micellar dispersion system; weigh 11.5962g of (C 6 h 5 ) 3 SbBr 2 and 2.102g of SbS 2 Add to the above-mentioned micelle dispersion system, add the nitric acid of hydrolysis inhibitor 0.2mL, make (C 6 h 5 ) 3 SbBr 2 Slowly hydrolyzed, eventually in SbS 2 A thin layer of amorphous antimony oxide hydrate Sb is uniformly formed on the surface of 2 o 3 ×xH 2 O: The precursor was calcined at 500°C for 8 hours in an air atmosphere to form an ATO powder with a primary particle size of 7-15 nm and a secondary particle size of less than 100 nm. On this basis, the telecentric separation technology is applied to the preparation of ATO dispersion, replacing the traditional grid technology, so that ATO, dispersant and solvent can achieve high dispersion and high stability on the microscopic scale, and finally form a 60% high ATO nanocrystalline dispersion with solid content, such as image ...

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Abstract

The invention discloses a preparation method of a nanometer antimony doped tin oxide material and its high-solid-content dispersion. The preparation method comprises the following steps: preparing high-dispersion nano-ATO, adding a certain amount of a surfactant to a solvent, adding an antimony compound and a semi-soluble or insoluble inorganic tin compound according with a stoichiometric ratio into the above solvent, adding a hydrolysis inhibitor, stirring to slowly hydrolyze the antimony compound in order to uniformly form a thin layer of an amorphous antimony oxide hydrate on the surface of the tin compound and microscopically inhibit the agglomeration of an ATO precursor, and roasting at a proper temperature to finally form ATO powder with the primary particle size of 7-15nm and the secondary particle size of below 100nm. A centrifugation technology is applied to prepare an ATO dispersion, substitutes a traditional grating technology, and realizes the microscopic high dispersion and high stability of the ATO, a dispersant and the solvent, and the formed ATO nanocrystal dispersion with the high solid content of 30-80% can be widely applied in the fields of heat insulation coatings, antistatic plastics, fibers, solar cells and the like.

Description

technical field [0001] The invention relates to a preparation method of nano oxide material. In particular, it relates to a nano antimony-doped tin oxide material and a method for preparing the high-solid-content dispersion liquid thereof. Background technique [0002] At present, commonly used conductive materials such as graphite and various metal materials are opaque, while tin dioxide is a wide bandgap oxide semiconductor transparent to visible light, and it is also the first excellent transparent conductive material put into commercial use. To improve its conductivity and stability, it is often used for doping, such as SnO-Sb, SnO-F, etc. Because Sb 3+ Replaced part of Sn 4+ And the defect solid solution is formed, and the energy level difference between the "conduction band energy level" and the "valence band energy level" of the crystal is reduced after doping with antimony, so that the originally high resistivity of tin dioxide is displayed due to doping. propert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/00C09C3/06C09C3/08
Inventor 何丹农张春明王丹郑文陈超高林徐少洪
Owner SHANGHAI NAXU IND