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Liquid phase coprecipitation method for producing superfine tin indium oxide powder

A technology of indium tin oxide powder and co-precipitation, which is applied in chemical instruments and methods, inorganic chemistry, gallium/indium/thallium compounds, etc. It is beneficial to problems such as industrial production process, and achieves the effect of reducing agglomeration, easy control, and beneficial to industrial production.

Inactive Publication Date: 2009-10-21
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the metal tin is extremely unstable during the dissolution process, and it cannot completely guarantee that the metal tin dissolves into tetravalent tin ions, which affects the effect of tin doping, so that the prepared ITO powder has impurity
In the process of preparing ITO powder by this method, the hydrolysis and condensation operation units are not easy to control, which is not conducive to the industrial production process

Method used

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  • Liquid phase coprecipitation method for producing superfine tin indium oxide powder

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Experimental program
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Effect test

Embodiment 1

[0018] 1) 11.4 grams of 99.993% metallic indium are dissolved with 98wt% sulfuric acid to make the indium salt solution contain In 3+ The amount is 60g / l; the SnCl 4 ·5H 2 O dissolved in water to make a tin salt solution, containing Sn 4+ 50g / l; mix indium salt solution and tin salt solution according to In 2 o 3 :SnO 2 (wt%)=90%: 10%, obtain indium tin salt solution for subsequent use; 2) with (NH 4 ) 2 SO 4 and NH 3 ·H 2 O is used as raw material to prepare 250ml of pH=7.0 (NH 4 ) 2 SO 4 -NH 3 ·H 2 The O solution is used as the bottom liquid in the reactor, and the dehydrated alcohol of 6% (being 15ml) of the total volume of the bottom liquid is added in the bottom liquid; 4 ) 2 SO 4 -NH 3 ·H 2 In the O bottom liquid, the injection process controls the injection speed of indium tin salt solution and ammonia water to keep the pH of the bottom liquid ≈ 7.0 ~ 7.8, and uses a water bath to maintain the reaction temperature at 70 ± 5 ° C, and continuously stirs ...

Embodiment 2

[0020] The chemical composition of the raw materials is: 99.994% metal In, 98wt% sulfuric acid, analytically pure SnCl 4 ·5H 2 O, analytically pure (NH4) 2 · SO 4 , analytically pure 25 wt% NH 3 ·H 2O and analytically pure absolute ethanol. 1) 16.8 grams of 99.994% metallic indium are dissolved with 98% sulfuric acid to make the indium salt solution contain In 3+ The amount is 150g / l; the analytically pure SnCl 4 ·5H 2 O dissolved in deionized water to prepare a tin salt solution, containing Sn 4+ 100g / l; mix indium salt solution and tin salt solution according to In 2 o 3 :SnO 2 (wt%)=95%: 5% mix, obtain indium tin salt solution for subsequent use; 2) with (NH 4 ) 2 SO 4 and analytically pure 25% to 28wt% NH 3 ·H 2 O is the raw material preparation 500ml pH=8.0 (NH 4 ) 2 SO 4 -NH 3 ·H 2 The O solution is used as the bottom liquid in the reactor, and the dehydrated alcohol of 5% (being 25ml) of the bottom liquid total volume is added in the bottom liquid; I...

Embodiment 3

[0022] The chemical composition of the raw materials used is: 99.993% metal In, 65wt% nitric acid, analytically pure SnCl 4 ·5H 2 O, analytically pure (NH4) 2 · SO 4 , analytically pure 25 wt% NH 3 ·H 2 O and analytically pure absolute ethanol. 1) 18.4 grams of 99.993% metallic indium are dissolved with nitric acid to make the indium salt solution contain In 3+ The amount is 180g / l; the analytically pure SnCl 4 ·5H 2 O dissolved in deionized water to prepare a tin salt solution, containing Sn 4+ 150g / l; mix indium salt solution and tin salt solution according to In 2 o 3 :SnO 2 (wt%)=85%: 15% mixes and obtains indium-tin mixed salt solution for subsequent use; 2) with (NH 4 ) 2 SO 4 and NH 3 ·H 2 O is the (NH 4 ) 2 SO 4 -NH 3 ·H 2 The O solution is used as the bottom liquid in the reactor, and in the bottom liquid, add the dehydrated alcohol of 8% (being 16ml) of the bottom liquid total volume; Indium tin mixed salt solution and 20wt% ammoniacal liquor are ...

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Abstract

The invention relates to a method for preparing superfine indium tin oxide powder by liquid phase co-precipitation. In the present invention, metal indium, SnCl4 5H2O and ammonia water with a purity greater than 99.99% are used as raw materials, and (NH4)2SO4-NH3 H2O or NH4Cl-NH3 H2O solution with a pH of 7.0 to 9.0 is used as the reaction bottom liquid, and a certain amount of Absolute ethanol, using the liquid phase co-precipitation method to prepare the white indium tin hydroxide precursor, and then calcined to obtain the light yellow-green spherical ITO powder with an average particle size of 20-60nm. Since the pH of the reaction system is always kept in the range of 7.0 to 9.0, the complete simultaneous precipitation of indium ions and tin ions is guaranteed, and the agglomeration of colloidal particles caused by a wide range of pH changes is reduced. The process is reasonable, safe and easy to control. Conducive to industrialized production.

Description

1. Technical field: [0001] The invention relates to a method for producing superfine indium tin oxide powder by liquid phase co-precipitation, and belongs to the technical field of preparing indium tin oxide powder by hydrometallurgy technology. Two background technologies: [0002] Indium-Tin-Oxide (Indium-Tin-Oxide), referred to as ITO, is an important material of the indium system, and more than 70% of the world's indium is used to produce this material. ITO ultrafine powder material is a composite powder formed by doping a certain amount of tin oxide into indium oxide. It has a cubic ferromanganese crystal structure and is an n-type wide bandgap semiconductor with a bandgap width Eg=3.5eV. The wavenumber corresponding to the forbidden band width value is 2.8×10 4 cm -1 , the wavelength is 365nm. The ITO thin film made with it has a reflectivity of more than 70% for infrared rays, an absorption rate of 85% for ultraviolet rays, and a transmittance of more than 90% for ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G15/00
Inventor 杨斌徐宝强刘大春郭亚琴冯同春戴永年马文会邓勇李伟宏唐万启刘永成杨部正谢克强伍继君王飞
Owner KUNMING UNIV OF SCI & TECH
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