Pressureless sintering method for TFT-grade ITO target

A technology of atmospheric pressure sintering and target material, which is applied in the field of atmospheric pressure sintering of TFT-level ITO target materials, which can solve the problems of long production cycle, inability to obtain high-density ITO target materials, and easy delamination of the green body.

Active Publication Date: 2016-02-03
GUANGXI CRYSTAL UNION PHOTOELECTRIC MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patent CN201010597008.2 discloses a method for preparing ITO targets by pressureless sintering in an oxygen atmosphere. This method has a separate degreasing process. Compared with the present invention, the production cycle is long and high-density ITO cannot be obtained. target
However, if the molding method is used for molding, if the powder is not added with a molding agent, the molded body is prone to defects such as delamination, especially when molding TFT-level large-size ITO targets.

Method used

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  • Pressureless sintering method for TFT-grade ITO target

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 2.7kg of ultra-high activity ITO powder (particle size of powder is 80nm, purity is 99.995%, the highest single impurity component is 10ppm) after adding molding agent and granulated, and put it into a rectangular steel mold with a size of 264mm×347mm. Under the molding pressure of 30MPa, hold the pressure for 15 seconds with a hydraulic press to carry out compression molding. Put the molded blank into a flexible sheath, seal it and put it into a cold isostatic press, hold the pressure for 1200 seconds under a pressure of 180MPa, and perform cold isostatic pressing. Then put the green body formed by cold isostatic pressing into the sintering furnace for sintering. The sintering process is as follows: heat up to 100°C at a heating rate of 0.2°C / min, and hold for 1 hour; then raise the temperature to 250°C at a heating rate of 0.3°C / min, and hold for 4 hours; then raise the temperature at a heating rate of 0.2°C / min to 600°C, hold for 1 hour; then raise the tempera...

Embodiment 2

[0025] Weigh 7kg of ITO powder granulated by adding molding agent (the particle size of the powder is 60nm, the purity is 99.994%, and the single impurity component is up to 15ppm), and put it into a rectangular steel mold with a size of 264mm×850mm. Under the molding pressure of 50MPa, pressurize for 100 seconds with a hydraulic press to carry out compression molding. Put the molded blank into a flexible sheath, seal it and put it into a cold isostatic press, hold the pressure for 600 seconds under a pressure of 240 MPa, and perform cold isostatic pressing. Then put the green body formed by cold isostatic pressing into the sintering furnace for sintering. The sintering process is as follows: raise the temperature to 120 degrees at a heating rate of 0.5 degrees per minute, and keep it for 1.5 hours; then raise the temperature to 300 degrees at a heating rate of 0.6 degrees per minute, and keep it for 8 hours; then raise the temperature at a heating rate of 0.5 degrees per minu...

Embodiment 3

[0028] Weigh 12kg of ITO powder granulated by adding molding agent (the particle size of the powder is 100nm, the purity is 99.995%, and the single impurity component is up to 8ppm), and put it into a rectangular steel mold with a size of 480mm×860mm. Under the molding pressure of 50MPa, the hydraulic press is used to hold the pressure for 300 seconds to carry out compression molding. Put the molded blank into a flexible sheath, seal it and put it into a cold isostatic press, hold the pressure for 300 seconds under a pressure of 300 MPa, and perform cold isostatic pressing. Then put the green body formed by cold isostatic pressing into the sintering furnace for sintering. The sintering process is as follows: raise the temperature to 150 degrees at a heating rate of 1 degree / minute, and keep it for 2 hours; then raise the temperature to 350 degrees at a heating rate of 0.9 degrees / minute, and keep it for 10 hours; then raise the temperature at a heating rate of 0.9 degrees / minu...

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Abstract

The invention relates to a pressureless sintering method for a TFT-grade ITO target. The method includes the specific steps that ultra-high-activity ITO nanopowder is selected, the pelleted ITO powder is subjected to compression molding, the molding pressure ranges from 25 MPa to 80 MPa, and the holding time ranges from 15 seconds to 300 seconds; the ITO powder is subjected to isostatic cool pressing reinforcing, the isostatic pressing pressure ranges from 180 MPa to 300 MPa, and the holding time ranges from 300 seconds to 1,200 seconds; then the ITO power is directly placed in a sintering furnace, atmosphere is introduced, the ITO powder is divided into multiple segments for temperature rise and holding at certain temperature rise rate, and the ITO powder is cooled to room temperature at certain rate to complete sintering. The method is characterized in that the ITO powder pelleted by adding a molding agent is subjected to compression molding, and after isostatic cool pressing reinforcing, the ITO powder is directly placed in the sintering furnace to be sintered. Through the design of the sintering manufacturing procedure, an original degreasing process is fused into a sintering process, and the two processes are conducted in the sintering furnace together. Compared with the technology with the independent degreasing procedure, degreasing equipment is omitted, equipment investment is reduced, more energy is saved, the sintering period is shortened by about 40%, production efficiency is improved, and the method is suitable for mass production.

Description

technical field [0001] The invention relates to a sintering method of an ITO target material, in particular to a normal pressure sintering method of a TFT grade ITO target material. Background technique [0002] ITO (indium tin oxide) target is the raw material for preparing ITO transparent conductive film. Widely used in liquid crystal displays, touch screens, etc. China is a big consumer of ITO targets, but high-end TFT-grade ITO targets (mainly used in LCD TVs, computer displays, high-end smartphones, etc.) are almost entirely dependent on imports (the annual consumption of TFT-grade ITO targets in China is about 600 tons) . The main characteristics of TFT grade ITO targets are high density (relative density ≥ 99.7%), large size [the size of one side is (260-1100) mm], and small nodules after sputtering (after use, the target The surface of the material is smooth and free of particles), and the quality of the ITO film is high. At present, the international mainstream ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01C04B35/64
Inventor 黄誓成陆映东黄作武建良农浩
Owner GUANGXI CRYSTAL UNION PHOTOELECTRIC MATERIALS CO LTD
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