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Manufacturing method of advanced-generation TFT-grade fine-grain ITO target material

A manufacturing method and fine-grained technology, which is applied in metal material coating process, ion implantation plating, coating, etc., can solve the problems of lack of reach, large grain size of target material, uneven composition, etc., and achieve reduction Firing temperature, accurate composition ratio, and the effect of improving sintering activity

Pending Publication Date: 2021-04-30
韶关市欧莱高纯材料技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Chinese patent CN105294072B discloses a normal-pressure sintering method for TFT-grade ITO targets, in which the grain size index of the ITO targets is not controlled, and the maximum sintering temperature is 1550 to 1650 °C, and the temperature is kept for 4 to 12 hours. The target grain size is too large
This invention is produced by synthetic ITO powder. Compared with the two different particle sizes of indium oxide and tin oxide nano-powders of the present invention, it is difficult to accurately control the proportion of indium and tin, and the particle size matching of the two powders cannot be controlled separately.
[0006] Chinese patent CN105712719B discloses an atmospheric pressure sintering manufacturing method for a large-scale high-density fine-grained ITO target. The relative density of the prepared ITO target is above 99.5%, and the grain size is 6 to 10 μm. High-generation TFT-grade ITO targets require a relative density above 99.7%, and a grain size below 5 μm
[0007] Chinese patent CN107010940A discloses a method for preparing an ITO sputtering target for TFT-LCD by controlling the oxygen content. This invention only focuses on the control of the oxygen content of the ITO target, and does not describe and control the grain size index of the target.
The alloy gasification powder making process adopted by it has the risk of insufficient metal oxidation and uneven composition. In addition, sintering needs to be carried out under oxygen pressure atmosphere, which has high requirements for sintering equipment.

Method used

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  • Manufacturing method of advanced-generation TFT-grade fine-grain ITO target material
  • Manufacturing method of advanced-generation TFT-grade fine-grain ITO target material
  • Manufacturing method of advanced-generation TFT-grade fine-grain ITO target material

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Experimental program
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Effect test

Embodiment 1

[0070] In the powder preparation step, indium oxide nanopowder and tin oxide nanopowder are respectively prepared. The purity of the two powders is greater than 99.99%. The indium oxide powder and tin oxide powder are respectively calcined at 750°C and subjected to rapid cooling to obtain indium oxide nanopowder. and tin oxide nanopowder. The specific surface area of ​​indium oxide nanopowder BET = 14.2m 2 / g, the specific surface area of ​​tin oxide nanopowder BET=17.8m 2 / g. Weigh 22.5kg of indium oxide nanopowder and 2.5kg of tin oxide nanopowder with a balance, add them into pure water equipped with dispersant, adhesive, and defoamer, start the sand mill for grinding, and detect the particle size of the slurry D50 = 0.22μm , stop grinding, spray-dry and granulate, and detect the particle size of the granulated powder D50=10.4 μm. The granulated powder is molded with a mold of 2000mm*290mm under a pressure of 50MPa, and the pressure holding time is 90s. The density of t...

Embodiment 2

[0072] Indium oxide nanopowder and tin oxide nanopowder were prepared respectively. The purity of the two powders was greater than 99.99%. The indium oxide powder and tin oxide powder were respectively calcined at 825°C and subjected to rapid cooling. The specific surface area of ​​the indium oxide nanopowder was BET = 13.5m 2 / g, the specific surface area of ​​tin oxide nanopowder BET=16.7m 2 / g. Weigh 22.5 kg of indium oxide powder and 2.5 kg of tin oxide powder with a balance, add them into pure water equipped with dispersant, adhesive, and defoamer, start the sand mill to grind, detect the particle size of the slurry D50 = 0.24 μm, stop Grinding, spray-drying and granulating, the particle size of the granulated powder was detected as D50=10.8 μm. The granulated powder is molded with a mold of 1310*288mm under a pressure of 50MPa, and the holding time is 90s. The formed blank is sealed in a flexible sheath, and then pressed in an isostatic press with a pressure of 350MPa a...

Embodiment 3

[0074] Indium oxide nanopowder and tin oxide nanopowder were prepared respectively. The purity of the two powders was greater than 99.99%. The indium oxide powder and tin oxide powder were respectively calcined at 850°C and subjected to rapid cooling. The specific surface area of ​​the indium oxide nanopowder was BET = 12.5m 2 / g, the specific surface area of ​​tin oxide nanopowder BET=18.6m 2 / g. Weigh 27kg of indium oxide powder and 3kg of tin oxide powder with a balance, add them into pure water equipped with dispersant, adhesive, and defoamer, start the sand mill for grinding, detect the slurry particle size D50=0.24 μm, stop grinding, Spray-dried and granulated, the particle size of the granulated powder was detected as D50=11.6 μm. The granulated powder was put into a tubular silicone flexible sheath and sealed, and then pressed in an isostatic press with a pressure of 380 MPa and a holding time of 600 s. The density of the biscuit was measured to be 62.6%. Put the bla...

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Abstract

The invention discloses a manufacturing method of an advanced-generation TFT fine-grain ITO target material. The manufacturing method comprises a powder preparation step, a mixing and grinding step, a spray granulation step, a compression molding step and a sinter molding step. According to the manufacturing method of the ITO target material, the ITO target material with large-size and high-density crystal grains can be manufactured, the density of the target material is larger than 99.9%, and the average crystal grain diameter is controlled to be 3-5 [mu]m.

Description

technical field [0001] The invention relates to the technical field of ITO target material manufacturing, in particular to a manufacturing method of high-generation TFT grade fine-grain ITO target material. Background technique [0002] Indium tin oxide target, referred to as ITO target, is a mixture of two metal oxides, indium oxide and tin oxide, which is sintered at high temperature to form a ceramic functional material. The ITO target material sintered with tin oxide doped indium oxide can form an ITO transparent conductive film on transparent substrates such as glass after vacuum magnetron sputtering coating, which is a necessary key material for the liquid crystal display panel industry. [0003] At present, the feasible sintering methods for ITO target production include hot pressing, hot isostatic pressing, pressure atmosphere sintering and atmospheric pressure sintering. The forming of the blank before the target sintering includes slip casting, compression molding...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01C04B35/622C23C14/34C23C14/35
CPCC04B35/01C04B35/622C04B2235/3293C04B2235/602C04B2235/6562C04B2235/6565C04B2235/6567C04B2235/658C04B2235/6585C04B2235/661C04B2235/77C04B2235/786C23C14/3414C23C14/35
Inventor 李鹏文宏福
Owner 韶关市欧莱高纯材料技术有限公司
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