Preparation method of solid spherical ITO granulation powder

A granulated powder and spherical technology, which is applied in the field of preparation of solid spherical ITO granulated powder, can solve the problems of difficulty in taking into account, inability to obtain high-quality target materials, complicated preparation method and process flow, etc.

Inactive Publication Date: 2020-10-23
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Abstract
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Problems solved by technology

Granulation technology is a core technology of dry molding. The prepared granulated powder must have good mold filling and fluidity and few defects. In order to meet this requirement, the granulated powder is usually required to be solid spherical. However, the current The ITO granulated powder prepared with advanced technology is generally in the shape of a hollow apple, so that it is impossible to obtain high-quality targets
[0004] The preparation of solid spherical granulated powder requires the slurry to have a high viscosity, but in order to ensure that the ITO powder is fully ground, a dispersant is usually added to reduce the viscosity of the slurry. Therefore, in actual production, it is difficult to take both into account. Solid spherical granulated powder
The Chinese patent with the publication number CN106082993A crushes and disperses the ITO powder after granulation, and performs secondary granulation to obtain solid spherical granulation. However, the preparation method process is relatively complicated, which virtually increases the production cost.

Method used

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  • Preparation method of solid spherical ITO granulation powder

Examples

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preparation example Construction

[0027] A method for preparing solid spherical ITO granulated powder, selecting indium oxide powder with a particle size of 10-500nm and tin oxide powder with a particle size of 10-500nm, and mixing the indium oxide powder and tin oxide powder at a mass ratio of 9:1 Add deionized water to make a slurry with a solid content of 50-80%, and then add a dispersant accounting for 0.1-5% of the total powder mass to it and grind thoroughly. The particle size of the slurry after grinding satisfies D90=0.1-2µm, Then add a binder accounting for 1-10% of the total powder mass to the slurry and mix evenly, then heat the slurry or adjust the pH value of the slurry to control the viscosity of the slurry at 100-1500mPa·s, and finally adjust the slurry Carry out spray drying to ensure that the inlet air temperature is 100~300°C, the outlet air temperature is 60~200°C, and the atomizer frequency is 20~50Hz, that is, the solid spherical ITO granulated powder with a particle size of 20~150µm is obt...

Embodiment 1

[0032] A preparation method of solid spherical ITO granulated powder, the steps are as follows:

[0033] Weigh 9Kg indium oxide powder, 1Kg tin oxide powder, indium oxide powder D50=125nm, tin oxide powder D50=88nm, add 6Kg deionized water to make slurry, then add 0.06Kg polycarboxylic acid dispersant to it, Grind with a sand mill for 2h, the slurry D90=0.6μm. Weigh 0.15Kg of polyvinyl alcohol, add it to the slurry, disperse evenly, heat the slurry to 75°C, and check the viscosity in real time. When the viscosity is 500mPa·s, stop heating. Put the slurry into the spray drying tower for spray drying, the inlet air temperature is 220°C, the outlet air temperature is 90°C, and the atomizer frequency is 35Hz.

[0034] The ITO granulated powder that this embodiment obtains is solid spherical, bulk density 1.91g / cm 3 , after 20MPa dry pressing and 200MPa isostatic pressing to obtain a green body, the relative density of the target obtained by sintering in an oxygen atmosphere is 9...

Embodiment 2

[0036] A preparation method of solid spherical ITO granulated powder, the steps are as follows:

[0037] Weigh 9Kg indium oxide powder, 1Kg tin oxide powder, indium oxide powder D50=50nm, tin oxide powder D50=20nm, add 8Kg deionized water to make slurry, then add 0.1Kg polyacrylamide dispersant to it, use Sand mill grinding 2h, slurry D90=0.3μm. Weigh 0.2Kg of polyethylene glycol, add the slurry, and disperse evenly. Add acetic acid to the slurry, adjust the pH to 5, the viscosity of the slurry is 400mPa·s, stop heating. Put the slurry into the spray drying tower for spray drying, the inlet air temperature is 200°C, the outlet air temperature is 80°C, and the atomizer frequency is 50Hz.

[0038] The ITO granulated powder that this embodiment obtains is solid spherical (as figure 1 shown), bulk density 1.78g / cm 3 , through 20MPa dry pressing and 200MPa isostatic pressing to obtain a green body, and the relative density of the target obtained by sintering in an oxygen atmosp...

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Abstract

The invention discloses a preparation method of solid spherical ITO granulation powder. The method comprises the following steps: preparing indium oxide powder and tin oxide powder into a slurry; adding a dispersing agent into the slurry, fully grinding, adding a binder, uniformly mixing, heating the slurry or adjusting the pH value of the slurry to control the viscosity of the slurry to be 100-1500mPa. S, and finally carrying out spray drying on the slurry to obtain the solid spherical ITO granulation powder. According to the preparation method, sufficient grinding and dispersing of the ITO granulation powder can be guaranteed, the solid spherical ITO granulation powder can be prepared, operation is convenient, and the requirement for high-performance target material preparation is met.

Description

technical field [0001] The invention relates to the field of indium tin oxide granulated powder, in particular to a preparation method of solid sphere ITO granulated powder. Background technique [0002] ITO film has good electrical conductivity and high visible light transmittance. It is a good transparent electrode material and is widely used in flat panel display, solar cell, electrochromic and other fields. At present, ITO thin films are mainly obtained by magnetron sputtering on ITO targets, and the quality of ITO targets determines the performance of the films. [0003] Dry molding is a commonly used molding method for preparing ITO targets, mainly molding-assisted isostatic pressing, or direct isostatic pressing molding process. Granulation technology is a core technology of dry molding. The prepared granulated powder must have good mold filling and fluidity and few defects. In order to meet this requirement, the granulated powder is usually required to be solid sphe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/626C04B35/453C04B35/01
CPCC04B35/62695C04B35/453C04B35/01C04B2235/3293C04B2235/32C04B2235/528C04B2235/77C04B2235/602C04B2235/6583C04B2235/5454C04B2235/5445
Inventor 师琳璞赵延飞薛建强杨硕
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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