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Method for preparing nano ITO powder by ammonia salt combustion method

A combustion method and nanotechnology, applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc., can solve the problems of long cycle, affecting target sintering, long time, etc., and achieve simple operation and short process flow , the effect of narrow particle size distribution

Inactive Publication Date: 2011-04-20
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although this method does not directly use chlorides for preparation, there is a process in this method that carries out hydrothermal reaction in a reactor at 130-260°C for 3-24 hours, and the time is too long, resulting in a long cycle of the entire reaction
CN1301911C discloses " a kind of ITO powder preparation method of solid-solution tin in indium oxide ", and it is to use indium nitrate and tin chloride mixed solution as raw material, utilizes spray pyrolysis method to prepare nanometer ITO powder, the powder that this method makes is Spherical, but because it contains chloride ions, it will also affect the sintering of the target

Method used

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  • Method for preparing nano ITO powder by ammonia salt combustion method
  • Method for preparing nano ITO powder by ammonia salt combustion method
  • Method for preparing nano ITO powder by ammonia salt combustion method

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1, take a certain amount of pure metal In10g, Sn1.1062g (weight ratio is In: Sn=9.04: 1) is dissolved in 63% HNO 3 1.2mol / L nitrate solution was prepared into 80ml concentration, and 10ml of organic complexing agent polyvinyl alcohol (the volume ratio to the solution was 1:8) and polyacrylamide 13.3ml (the volume ratio to the solution was 1:8) was added successively. 1: 6); then add dispersant citric acid 5.3g (the volume ratio with the solution is 1: 15), fructose 5.3g (the volume ratio with the solution is 1: 15) successively, stir constantly, the temperature is controlled at 45 ℃, After the complexing agent added and the dispersant were completely dissolved, ammoniacal liquor was added dropwise to adjust the pH value to 3.8, and in the obtained ammonium salt solution, 7.3ml of dehydrated alcohol was added with a solution volume ratio of 1: 11, as As a combustion aid, put it into a rotary kiln at 800°C and sinter for 10 minutes to obtain ITO powder.

Embodiment 2

[0020] Embodiment 2, take a certain amount of pure metal In10g, Sn1.1062g (weight ratio is In: Sn=9.04:1) is dissolved in 63% HNO 3 In, be configured into 60ml concentration and be the nitrate solution of 1.6mol / L, add organic complexing agent polyvinyl alcohol 5ml (the volume ratio with the solution is 1: 12) and polyacrylamide 7.5ml (the volume ratio with the solution is 1:12) successively 1: 8); then add dispersant citric acid 3.75g (the volume ratio with the solution is 1: 16), fructose 3.75g (the volume ratio with the solution is 1: 16) successively, stir constantly, the temperature is controlled at 60 ℃, After the added complexing agent and dispersant are completely dissolved, add ammonia water dropwise to adjust the pH value to 3.5, add 5ml of dehydrated alcohol with a solution volume ratio of 1:12 in the prepared ammonium salt solution, as a combustion aid agent, put it into a rotary kiln at 1000°C and sinter for 20 minutes to obtain ITO powder.

Embodiment 3

[0021] Embodiment 3, take a certain amount of pure metal In10g, Sn1.1062g (weight ratio is In:Sn=9.04:1) is dissolved in 63%HNO 3 50ml of nitrate solution with a concentration of 1.92mol / L was configured, and 3.6ml of organic complexing agent polyvinyl alcohol (the volume ratio of the solution was 1:14) and polyacrylamide 5ml (the volume ratio of the solution was 1:14) was added successively. 1: 10); then add dispersant citric acid 2.8g (the volume ratio with the solution is 1: 18), fructose 2.8g (the volume ratio with the solution is 1: 18) successively, stir constantly, the temperature is controlled at 70 ℃, After the complexing agent added and the dispersant were completely dissolved, ammoniacal liquor was added dropwise to adjust the pH value to 2.5, and in the obtained ammonium salt solution, 3.8ml of dehydrated alcohol was added with a solution volume ratio of 1:13, as Put the combustion aid into a rotary kiln at 1100°C and sinter for 30 minutes to obtain ITO powder.

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Abstract

The invention relates to a method for preparing nanometer ITO powder by means of ammonia salt combustion process, which comprises the following steps: metals of indium and tin are dissolved into nitric acid solution to prepare nitrate solution, organic complexing agent and dispersant are added into the resultant solution and mixed evenly, and the temperature is controlled between 40 and 70 DEG C; then ammonia water is added into the solution, and the pH value is adjusted between 1 and 3.8; finally, absolute ethyl alcohol is added into the prepared ammonia salt solution as combustion improver, liquid drops of the solution is dripped into a rotary kiln with a temperature of 700-1200 DEG C and sintered for 10 to 30 minutes, thus obtaining the nanometer ITO powder. The preparation method for nanometer ITO powder has the advantages that the powder produced has high purity and a grain size ranging between 10 and 30 nm, and the powder is of a regular spherical grain, and has no other impurities, especially chloridion; therefore, the problems of sever cracks occurring on the target material during the ITO target material preparation process by means of sintering method and hot isostatic pressing method due to the abundant chlorine in the ITO powder; moreover, the process cycle is short, the production efficiency is high, and continuous feeding and powder production are possible, thus realizing mass production and causing no pollution to the environment.

Description

technical field [0001] The invention relates to a preparation method of high-purity indium tin oxide nanometer powder, which belongs to a kind of wet method preparation of nanometer ITO powder. Background technique [0002] Indium Tin Oxide (Indium Tin Oxides, English abbreviation ITO) nanopowder refers to 90% In 2 o 3 with 10% SnO 2 The oxide material composed of it is a new type of special functional material and a high-tech product of deep processing of metal indium. ITO powder is mainly used to prepare ITO targets and ITO thin films. ITO film has high transmittance to visible light, high reflectivity in the infrared region, high absorption rate in the ultraviolet region, good electrical conductivity, good substrate adhesion and chemical stability. The above-mentioned characteristics of ITO make it widely used in many fields, and become a transparent conductive material with important application and research value at this stage. Usually, only high-quality ITO powder...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02C01G15/00
Inventor 竺培显陈敬超孙丽达李仲揆王勋业
Owner KUNMING UNIV OF SCI & TECH
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