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Method for preparing ITO (Indium Tin Oxide) granulation powder by mixing method

A technology of granulating powder and mixing method, which is applied in the field of preparation of ITO granulating powder, can solve the problems of dispersant failure, complicated operation, difficult to transfer clean, etc., and achieve the goal of reducing grinding time, avoiding particle agglomeration, and shortening grinding time Effect

Inactive Publication Date: 2020-05-12
洛阳晶联光电材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is more common in the world. The obtained powder has high sintering activity, small and uniform grain size, and is suitable for high-end TFT fields. However, there are certain problems: due to mechanical mixing, the mixing of indium oxide and tin oxide Uniformity is an important consideration factor. The uniformity of the two in the slurry determines the uniformity of the target. The usual method is to prolong the ball milling time, but too long milling will cause the dispersant to fail and agglomerate, and the surface of the powder particles Disadvantages such as reduced activity due to long-term mechanical friction
[0006] Chinese patent 201610400659.5 discloses a method for preparing high-performance ITO granulated powder, which still adopts the same feeding sequence as the existing mechanical mixing method in the preparation process, that is, first put indium oxide, tin oxide, and dispersant in the mixing tank Make a slurry, and then grind it to a certain size in a ball mill, then add a binder to grind for a period of time, after spray drying the first granulation, you need to add a dispersant for high-speed dispersion, and then carry out secondary granulation by spray drying. Although the activity of the powder is improved to a certain extent, the operation is complicated and needs to be carried out in different material barrels, and the material needs to be transferred multiple times, that is, the material needs to be transferred from the mixing tank to the ball mill, and from the ball mill to the spray drying device. The transfer of materials from the high-speed dispersing device to the spray drying device is very troublesome in actual operation, and the transfer of materials will actually waste a lot of time; and in different machines, the materials will definitely stick a lot inside, making it difficult to transfer cleanly. cause material waste

Method used

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  • Method for preparing ITO (Indium Tin Oxide) granulation powder by mixing method
  • Method for preparing ITO (Indium Tin Oxide) granulation powder by mixing method
  • Method for preparing ITO (Indium Tin Oxide) granulation powder by mixing method

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Effect test

Embodiment 1

[0033] Embodiment 1: Get 90Kg of indium oxide powder and 10Kg of tin oxide powder, the average grain size of indium oxide powder is 120nm, the average grain size of tin oxide powder is 70nm, standby; Get 0.5Kg of polycarboxylic acid compound Dispersant and 1.5Kg of polyvinyl alcohol are dissolved in deionized water to form a mixed solution of 40Kg, the weighed powder is added to the mixed solution, and a pre-dispersed slurry with a solid content of 71.4% is prepared under stirring; Put the slurry into an ultrasonic instrument with an ultrasonic frequency of 40 Hz for 30 minutes, then add it to a sand mill and grind it for 1 hour. When the corresponding slurry particle size D50 is 0.5 micron and D90 is 1 micron, add a few drops of n-butanol to Defoaming to prepare a mixed slurry, spray drying to obtain ITO granulated powder, wherein the inlet air temperature is 220°C, the outlet air temperature is 100°C, and the atomizer frequency is 30Hz.

[0034] Comparative test 1 (the steps...

Embodiment 2

[0038] Embodiment 2: Get 90Kg of indium oxide powder and 10Kg of tin oxide powder, the average grain size of indium oxide powder is 100nm, the average grain size of tin oxide powder is 100nm, standby; Get 0.7Kg of polyvinylpyrrolidone dispersant Dissolve carboxymethyl cellulose and 1.5Kg in deionized water to form a mixed solution of 40Kg, add the weighed powder into this mixed solution, and make a pre-dispersed slurry with a solid content of 71.4% under stirring; Put the slurry into an ultrasonic instrument with an ultrasonic frequency of 40 Hz for 30 minutes, then add it to a sand mill and grind it for 1 hour. When the corresponding slurry particle size D50 is 0.4 micron and D90 is 0.9 micron, add a few drops of n-butanol to Defoaming to prepare a mixed slurry, spray drying to obtain ITO granulated powder, wherein the inlet air temperature is 180°C, the outlet air temperature is 80°C, and the atomizer frequency is 35Hz.

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Abstract

The invention relates to a method for preparing ITO (indium tin oxide) granulation powder by a mixing method. The method comprises the following steps: (1) weighing indium oxide and tin oxide powder for later use; (2) dissolving a dispersing agent and a binder in deionized water; (3) dispersing indium oxide and tin oxide powder into the solution obtained in the step (2); (4) putting the slurry into an ultrasonic instrument for pre-dispersion to obtain slurry to be ground; (5) putting the slurry to be ground into a ball mill for grinding; (6) adding a defoaming agent into the slurry, and stirring for defoaming; and (7) carrying out spray drying on the mixed slurry to obtain the ITO granulation powder. According to the method, by adding all materials and additives (the dispersing agent and the binder) at the same time, pre-dispersing the slurry under the combined action of ultrasonic treatment and stirring and putting the slurry into a grinding machine for sanding, the advantages that the grain size of the target material is small and uniform can be obtained through a mechanical mixing method, and the problem that good component uniformity and high activity are difficult to obtain atthe same time when ITO particles are prepared through a mixing method is solved.

Description

technical field [0001] The invention belongs to the technical field of indium tin oxide composite powder preparation, and relates to a method for preparing ITO granulated powder by a powder mixing method, in particular to a method for preparing ITO granulated powder with high uniformity and high activity. Background technique [0002] The ITO target is an important raw material for the preparation of ITO conductive glass. Usually, the ITO target is prepared into an ITO film by magnetron sputtering. Its performance is the key factor determining the quality, production efficiency and yield of conductive glass products. The quality of the ITO granulated powder is an important factor determining the performance of the ITO target, and the ITO granulated powder is required to have high purity, good activity, and uniformity. [0003] The main methods for preparing ITO powder include mechanical mixing method, spray pyrolysis method, sol-gel method, hydrothermal synthesis method, co-...

Claims

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Application Information

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IPC IPC(8): C04B35/626C04B35/453
CPCC04B35/453C04B35/6261C04B35/62695C04B2235/5436C04B2235/5445C04B2235/5454C04B2235/77
Inventor 史海月陈志强郭朋马闯
Owner 洛阳晶联光电材料有限责任公司
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