Method for preparing high-compact ITO target material through two-step sintering

A segmental sintering and target technology, which is applied in the field of high-density ITO target preparation by sintering method, can solve the problems of high equipment cost, influence of target coating performance, uneven microstructure, etc., and improve strength and thermal shock resistance , Uniform strength and microstructure, avoiding the effect of abnormal grain growth

Active Publication Date: 2017-07-25
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method needs to control and adjust many parameters such as the specific surface area of ​​the nano-powder, the pH value of the slurry, and the viscosity, and the green body takes a long time to dry and degrease, which requires high pulping technology, is not easy to operate, has a low yield, and is prone to needles. Pore ​​defects, resulting in increased nodules during the coating process
[0007] CN103232234 A discloses a method for microwave doping sintering, in which additives such as ZnO and TiN are added, which will introduce more impurities, which will affect the coating performance of the target
Moreover, although the temperature of microwave sintering is low, microwave sintering leads to uneven internal microstructure, and deformation and cracking are prone to occur during the sintering process. Due to equipment limitations, the output is not as large as that of normal pressure sintering, and the equipment cost is high.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027]Example 1: Indium oxide with an average particle diameter of 200nm and tin oxide with an average diameter of 100nm were weighed at a mass ratio of 90:10, and a certain amount of water was added to prepare a slurry with a concentration of 45% by mass. Then add 0.8% powder mass percentage of dispersant ammonium polyacrylate for ball milling for 8 hours, then add 2% powder mass percentage of binder polyvinyl alcohol for ball milling for 3 hours. After uniform ball milling, the slurry is sprayed and granulated to obtain granulated powder. Under a pressure of 30MPa, take an appropriate amount of granulated powder and press it into a green body under a steel mold, and then isostatically press it under a pressure of 250MPa to obtain a green body. Take the biscuit and degrease it at 500°C for 20 hours in an air atmosphere, then raise the temperature to 1000°C at a rate of 100°C / h, keep it warm for 10 hours, and then cool with the furnace to complete the first step of pre-firing....

Embodiment 2

[0028] Example 2: Take indium oxide with an average particle size of 100nm and tin oxide with an average particle size of 70nm, weigh them with a mass ratio of 90:10, add a certain amount of water to make a slurry with a mass percentage of 50%, and add 2% powder mass Percentage dispersant ammonia water was ball milled for 8 hours, and then 1% powder mass percentage of binder polyethylene glycol was added for ball milling for another 2 hours, and then the slurry was sprayed and granulated to obtain granulated powder. Then take an appropriate amount of granulated powder and press under a steel mold with a pressure of 16MPa to form a green body, and then isostatically press under a pressure of 300MPa to obtain a green body. Take the biscuit and degrease it at 500°C for 20 hours in an air atmosphere, then raise the temperature to 1100°C at a rate of 100°C / h, keep it warm for 20 hours, and then cool with the furnace to complete the first step of pre-firing. The pre-fired green body...

Embodiment 3

[0029] Example 3: Take indium oxide with an average particle diameter of 200nm and tin oxide with an average particle diameter of 70nm, and add a certain amount of water at a mass ratio of 90:10 to prepare a slurry with a concentration of 50% by mass. Add 1.5% powder mass percentage of dispersant ammonium polyacrylate and ball mill for 10 hours, then add 2.5% powder mass percentage of binder polyvinyl butyral for ball milling for 3 hours, and then spray granulate to obtain granulated powder. Take the granulated powder and press it into a green body in a steel mold of 36MPa, and then isostatically press at 280MPa to obtain the final green body. Take the green body and degrease it in the air furnace at 500°C for 20 hours, then raise the temperature to 800°C at a rate of 100°C / h, keep it warm for 30 hours, and then cool with the furnace to complete the first step of pre-firing. The pre-fired green body is placed in an oxygen atmosphere sintering furnace, and a corundum mullite ca...

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Abstract

The invention discloses a method for preparing a high-compact ITO target material through two-step sintering. The method comprises the following steps: firstly manufacturing the raw material into a biscuit, keeping warm and degreasing under the air atmosphere, directly placing under the air atmosphere to warm to 800-1300 DEG C after the degreasing and keeping warm for 5-30 hours to perform the first step of pre-sintering; placing the pre-sintered green body on a sintering bearing plate, warming to 1500-1600 DEG C and keeping warm for 5-30 hours under the oxygen atmosphere so as to perform the second step of sintering; stopping introducing the oxygen 1-5 hours before finishing the sintering; and performing furnace cooling to obtain an ITO target sintering body. The pre-sintering is performed under the air atmosphere so that the sintering time of the oxygen atmosphere can be shortened, the production energy consumption is greatly lowered; the degreasing and the pre-sintering process are integrated so that the sintering total time is saved; the pre-sintering enables the particles in the green body to be further homogenized, the abnormal crystal grain growth is avoided, and the microscopic homogeneity of the target is improved, and the strength and the thermal shock resistance are improved; the prepared ITO target density reaches to 7.128g/cu.cm and more.

Description

technical field [0001] The invention relates to a method for preparing an ITO target material, in particular to a method for preparing a high-density ITO target material by a sintering method. Background technique [0002] ITO (Tin-doped Indium Oxide) target belongs to indium-tin composite oxide ceramics, which is often used as a magnetron sputtering target to prepare transparent conductive films on glass, plastic and other substrate materials for the production of flat panel display devices such as liquid crystal displays and touch screens . Currently published ITO target sintering methods include oxygen pressure sintering, pressureless sintering, SPS sintering, hot pressing sintering, hot isostatic pressing sintering, microwave sintering, etc. Most of the sintering technologies of ITO targets have one or more problems such as high sintering temperature, long sintering time, high powder processing requirements, difficult slurry preparation, adding sintering aids or requiri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/01C04B35/64
CPCC04B35/01C04B35/64C04B2235/3293C04B2235/5445C04B2235/5454C04B2235/602C04B2235/656C04B2235/6562C04B2235/6567C04B2235/658C04B2235/6583C04B2235/661C04B2235/77C04B2235/786C04B2235/96
Inventor 许亚利方宏刘冠鹏崔晓芳
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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