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Preparation method of evaporation ITO particle and ITO particle prepared through preparation method

A granule, press-forming technology, applied in the field of ITO granules, can solve the problems of small gas flow, large temperature difference in the furnace, and hidden quality problems in mass production of ITO granules, and achieve the effect of reducing gas consumption, fully decomposing and reacting

Active Publication Date: 2018-05-08
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The former adopts a high-temperature sintering furnace with ordinary electric heating and can pass through oxidizing gas. The equipment is simple, but the oxygen content in the atmosphere cannot be controlled or detected during the sintering process, and the product quality (such as oxygen loss rate, etc.) of ITO evaporated particles cannot be guaranteed. The equipment is controllable. The accuracy is poor; in addition, the normal pressure sintering furnace has a large furnace, the gas flow rate is small, and the temperature difference in the furnace is large, which has a great influence on the density and microstructure (such as grain size, etc.) of ITO particles. Therefore, the normal pressure sintering method The mass production of ITO particles brings quality hidden dangers
The latter can solve the problem of oxygen partial pressure, and can also solve the problem of uniformity of furnace temperature, but the biggest problem is that the sintering furnace is under pressure, which poses a hidden danger to production safety; in addition, the investment in equipment is larger than that of normal pressure sintering furnace, which is not conducive to control Cost of production

Method used

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  • Preparation method of evaporation ITO particle and ITO particle prepared through preparation method
  • Preparation method of evaporation ITO particle and ITO particle prepared through preparation method
  • Preparation method of evaporation ITO particle and ITO particle prepared through preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] as per figure 1 As shown in the technological process, weigh 9500 grams of In 2 o 3 Powder (average particle size 65nm, BET 12.80m 2 / g), 500 grams of SnO 2 Powder (average particle size 70nm, BET 12.50m 2 / g), 3586 gram of pure water and 200 gram of dispersants mix to make slurry, dispersant is the aqueous solution of polyacrylate, and its massfraction is 40wt%; Slurry is packed in the ball mill, press slurry and ball Load ZrO with a mass ratio of 1:2 2 Ball, rolling speed 50 rpm, ball milling time 12h; add 600 grams of binder and stir for 60 minutes, then spray granulation, the binder is an aqueous solution of polyvinyl alcohol, and its mass fraction is 10wt%; put ITO powder into In a steel mold or cemented carbide mold with a diameter of 27.5mm, hold the pressure at 25MPa for 1min to press into a disc-shaped ITO green body; put the ITO green body into a pressureless oxygen atmosphere sintering furnace, and first heat it at 60°C / Heating to 200°C at a heating ra...

Embodiment 2

[0041] The preparation of the ITO green body is the same as in Example 1. The ITO green body is put into a pressureless oxygen atmosphere sintering furnace, heated to 200 °C at a heating rate of 100 °C / h, and then heated to 600 °C at a heating rate of 30 °C / h. ℃ for 1h, the oxygen flow rate is 50L / min; then heated to 1400°C at a heating rate of 200°C / h for pressureless oxygen sintering, the sintering time is 5h, the oxygen flow rate is 50L / min; the finally obtained ITO particles are intact, the color It is light green, with a purity of 99.99%, and a relative density of 55.8% obtained by the size method. Through XRD detection, the phase structure is an indium oxide single-phase structure, and the cross-sectional SEM shows that the grain size is 5-10 μm.

Embodiment 3

[0043] Weigh 9800g In 2 o 3 Powder (average particle size 60nm, BET 13.60m 2 / g), 200 grams of SnO 2 Powder (average particle size 85nm, BET 10.35m 2 / g), 3586 grams of pure water and 200 grams of dispersant are packed into the ball mill, and the ITO green body is made by the ball mill mixing, granulation, and molding methods in Example 1, and the ITO green body is packed into a sintering furnace without pressure oxygen atmosphere. In, sintering is carried out by the degreasing sintering method in Example 1. The prepared ITO particles are intact, the color is light green, the purity is 99.99%, and the relative density is 61.7% according to the size method. Through XRD detection, the phase structure is an indium oxide single-phase structure, and the cross-sectional SEM shows that the grain size is 5-8 μm.

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Abstract

The invention provides a preparation method of an evaporation ITO particle. The method comprises the following steps performed in a non-pressure sintering furnace: (1) heating an ITO green body in anoxygen flowing environment to 180-240 DEG C at the heating speed of 10-100 DEG C per hour, then heating to 400-600 DEG C at the heating speed of 10-30 DEG C per hour, and preserving the heat for 1-4 hours after finishing heating; (2) heating in the oxygen flowing environment to 1300-1500 DEG C at the heating speed of 100-200 DEG C per hour, and conducting non-pressure oxygen sintering, wherein thesintering time is 1-10 hours. The preparation method simplifies the control conditions for the preparation of a powder, is favorable for separately controlling the quality of the powder, simplifies the forming, degreasing and sintering process, and is the first case among the domestic preparation methods of the ITO particle. The invention also provides the ITO particle. The ITO particle meets thetechnical requirements of the vacuum evaporation method, is uniform in structure, and does not crack easily.

Description

technical field [0001] The invention belongs to the technical field of semiconductor material preparation, and in particular relates to a method for preparing ITO particles used for preparing transparent conductive films by vapor deposition and the ITO particles prepared by the method. Background technique [0002] There are many methods for producing transparent conductive thin film materials, among which magnetron sputtering is the most widely used method. The magnetron sputtering method is mainly used in the manufacture of LCD and solar cell thin film materials. Because in the production process of semiconductors, the use of magnetron sputtering will cause serious damage to the semiconductor surface, so in the preparation of semiconductor light-emitting diodes (LEDs), organic light-emitting diodes (OLEDs), polymer light-emitting diodes (PLEDs) ) transparent conductive film, the method of vacuum evaporation coating is generally used. [0003] Vacuum evaporation coating i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G19/00
CPCC01G19/00C01P2002/72C01P2004/03C01P2004/62C01P2004/82C01P2006/10
Inventor 梅方胜蒋少英陈立三彭小苏赵为上
Owner ZHUZHOU SMELTER GRP
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