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Preparation of ito powder for rotating target by thermal spraying method and its production method and application

A production method, thermal spraying technology, applied in the direction of tin oxide, etc., can solve the problems of uneven etching of the target surface, low powder yield, poor fluidity, etc., to improve uniformity and sintering performance, inhibit nodule growth, Effect of improving electrical conductivity

Active Publication Date: 2017-04-19
ZHUZHOU SMELTER GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, a large number of flat target materials are mainly used in the market, and there are several difficult problems in the flat target materials: low target utilization rate (less than 40%); low coating power, low deposition rate of the film during sputtering, and low target surface Etching is uneven, and nodules are easy to form on the target surface, especially at the splicing part of the target, due to the influence of tip discharge, metal solder and target surface deposits, nodules are easily formed, resulting in instability of the coating process and affecting the quality of the coating ; And regular cleaning of target surface nodules will greatly reduce the production efficiency of coating
[0008] Some manufacturers directly use ITO powder prepared by chemical method to prepare rotating targets by thermal spraying. Due to the small powder particles, serious agglomeration, and poor fluidity, the prepared targets have low density and poor coating effect. At the same time, the utilization rate of ITO powder is also very low, greatly increasing the cost of preparation
Some manufacturers also use the sintered ITO block target for mechanical crushing to obtain a powder with a suitable particle size distribution, which is then used for thermal spraying to make a target. Although the powder obtained by this method can prepare a high-density rotating target, the broken The high content of impurities brought in the process will affect the quality of the film, and it is difficult to control the particle size of the powder during the crushing process, the yield of the powder is low, and the production cost is high

Method used

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  • Preparation of ito powder for rotating target by thermal spraying method and its production method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) Dissolve metal indium with hydrochloric acid into an indium salt solution, add tin tetrachloride salt according to the weight ratio of indium oxide: tin oxide 90:10, stir evenly, add ammonia water as a precipitant, and generate an ITO precursor. Washing, drying, and calcining at 800°C for 4 hours to obtain ITO coprecipitated powder;

[0042] (2) Add a certain amount of pure water to the obtained ITO co-precipitation powder, add 0.1% polyethylene glycol as a dispersant, and put it into a rolling ball mill for ball milling for 15 hours. The particle size of the slurry is 0.1~1.0 μm, and the ball milling is completed Finally, add 1% binder (polyvinyl alcohol) and stir evenly, and use the centrifugal spray granulation method for granulation. The particle size range of the obtained granulated powder is 30-120 μm.

[0043] (3) Put the granulated powder obtained by granulation into a calciner, heat up to 600°C at a rate of 30°C / h for degreasing, keep the degreasing for 1 h...

Embodiment 2

[0046] Example 2: The ITO granulated powder prepared by the method in Example 1 was heated to 600°C at a rate of 30°C / h for degreasing, kept for 1 hour for degreasing, and then heated to 1450°C at a rate of 200°C / h Sintering, sintering and heat preservation for 4 hours.

[0047] The sintered powder is put into a reduction furnace, and a hydrogen-nitrogen mixed gas with a hydrogen content of 20% is introduced, and the reduction treatment is carried out at 500°C, and the reduction degree is controlled at 1.5%, to obtain ITO powder with a purity of 99.99%.

[0048] 35 kg of the powder was used for thermal spraying to prepare an ITO rotating target, and a target material of 28.7 kg was obtained, the relative density of the target material was 96%, and the yield of the powder was 82%.

Embodiment 3

[0049] Example 3: The ITO precursor obtained by the method of Example 1 was washed, dried, and calcined at 1100°C for 4 hours, then 0.5% polyacrylamide was added as a dispersant, and ball milled to obtain a slurry with a particle size of 0.2 ~2.0μm, add polyvinyl alcohol as a binder for spray granulation, the particle size is 30~150μm. Put the granulated powder obtained by granulation into a calciner, heat up to 600°C at a rate of 30°C / h for degreasing, degrease and keep for 1 hour, then heat up to 1300°C at a rate of 200°C / h for sintering, sintering and heat preservation 4 hours. The sintered powder is put into a reduction furnace, and a hydrogen-nitrogen mixed gas with a hydrogen content of 20% is introduced, and the reduction treatment is carried out at 500°C, and the reduction degree is controlled at 1.5%, to obtain ITO powder with a purity of 99.99%.

[0050] 35 kg of the powder was used for thermal spraying to prepare an ITO rotating target, and a target material of 28....

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Abstract

The invention discloses ITO (indium tin oxide) powder for a rotating target prepared by a thermal spraying method as well as a production method and application of the ITO powder. The production method comprises the steps of adopting a wet-chemical method to prepare ITO co-precipitation powder, performing wet grinding distributed processing, performing spray granulation to obtain granulation powder, performing degreasing and sintering on the granulation powder, and performing reduction treatment to obtain the ITO powder. The ITO powder prepared by the method has good fluidity, better intensity and good sintering character, is not liable to be broken by air flow during a thermal spraying method process, is beneficial for improving the yield of powder during a preparation process, and is suitable for preparing the rotating target by directly using the thermal spraying method, and the density and target film coating quality of a thermal spraying target are ensured. The ITO powder is the ITO powder obtained through the production method, and the ITO powder obtained through the production method is used for preparing the rotating target by the thermal spraying method.

Description

technical field [0001] The invention relates to an ITO target material, a preparation method thereof and a product thereof, in particular to a thermal spraying method for preparing ITO powder for a rotating target, a production method and application thereof. Background technique [0002] The ITO target is indium tin oxide, which is an important raw material for preparing ITO thin films. ITO film is widely used in liquid crystal display (LCD) panel, touch sensor panel (Touch Panel), organic light-emitting flat-panel display (Organic ELD Panel), plasma display (PDP Panel), Automotive heat-proof and defogging glass, solar cells, photoelectric converters, anti-static films for transparent heaters, infrared radiation devices and other fields, among which the most important application field is the LCD industry. [0003] At present, a large number of flat target materials are mainly used in the market, and there are several difficult problems in the flat target materials: low ta...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G19/02C04B35/453C04B35/626
CPCC01G19/02C01P2004/01C01P2006/80C04B35/453C04B35/626C04B2235/3293
Inventor 彭小苏杨扬傅清波陈立三赵为上梅方胜杨岳云
Owner ZHUZHOU SMELTER GRP
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