阅读说明：本技术 一种实心球形ito造粒粉的制备方法 (Preparation method of solid spherical ITO granulation powder ) 是由 师琳璞 赵延飞 薛建强 杨硕 于 2020-06-23 设计创作，主要内容包括：本发明公开了一种实心球形ITO造粒粉的制备方法,先将氧化铟粉末和氧化锡粉末制成浆料,之后向其中加入分散剂并研磨充分、加入粘结剂并混合均匀,然后加热浆料或调节浆料的pH值使浆料的粘度控制在100~1500mPa·s,最后对浆料进行喷雾干燥即制得实心球形的ITO造粒粉。该制备方法既能保证ITO造粒粉的充分研磨和分散,又能制备出实心球形的ITO造粒粉,且操作方便,满足高性能靶材制备的要求。(The invention discloses a preparation method of solid spherical ITO (indium tin oxide) granulation powder, which comprises the steps of preparing indium oxide powder and tin oxide powder into slurry, adding a dispersing agent into the slurry, fully grinding the slurry, adding a binder into the slurry, uniformly mixing the binder and the slurry, heating the slurry or adjusting the pH value of the slurry to control the viscosity of the slurry to be 100-1500 mPa.s, and finally performing spray drying on the slurry to obtain the solid spherical ITO granulation powder. The preparation method can ensure the sufficient grinding and dispersion of the ITO granulated powder, can also prepare the solid spherical ITO granulated powder, is convenient to operate, and meets the requirement of high-performance target preparation.)

1. A preparation method of solid spherical ITO (indium tin oxide) granulation powder is characterized by mixing indium oxide powder, tin oxide powder and deionized water to prepare slurry, then adding a dispersing agent into the slurry, fully grinding the slurry, adding a binder into the slurry, uniformly mixing the binder and the slurry, then heating the slurry or adjusting the pH value of the slurry to control the viscosity of the slurry to be 100-1500 mPa.s, and finally performing spray drying on the slurry to obtain the solid spherical ITO granulation powder.

2. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: the specific operation of heating the slurry is as follows: and heating the slurry to 50-100 ℃, detecting the viscosity of the slurry in real time, and stopping heating when the viscosity of the slurry reaches the target viscosity.

3. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: the concrete operation of adjusting the pH value of the slurry is as follows: and adding any one of acetic acid, nitric acid or hydrochloric acid into the slurry to ensure that the pH of the slurry is less than 6.

4. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: selecting indium oxide powder with the particle size of 10-500 nm and tin oxide powder with the particle size of 10-500 nm, and adding the indium oxide powder and the tin oxide powder into deionized water according to the mass ratio of 9:1 to prepare slurry with the solid content of 50-80%.

5. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: the amount of the added dispersing agent is 0.1-5% of the total mass of the powder, and the dispersing agent is any one or the combination of more than two of polyacrylamide, polycarboxylic acid, polyacrylic acid, polyvinyl alcohol and polyethylene glycol.

6. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: after the dispersing agent is added into the slurry and fully ground, the particle size of the slurry meets D90= 0.1-2 mu m.

7. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: the amount of the added binder is 1-10% of the total mass of the powder, and the binder is any one or the combination of more than two of polyvinyl alcohol, polyethylene glycol, polyacetal and polymethyl cellulose.

8. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: during spray drying, the air inlet temperature is 100-300 ℃, the air outlet temperature is 60-200 ℃, and the frequency of the atomizer is 20-50 Hz.

9. The method for preparing solid spherical ITO granulating powder according to claim 1, wherein the method comprises the following steps: the particle size of the prepared ITO granulated powder is 20-150 mu m.

Technical Field

The invention relates to the field of indium tin oxide granulation powder, in particular to a preparation method of solid spherical ITO granulation powder.

Background

The ITO film has good conductivity and high visible light transmittance, is a good transparent electrode material, and is widely applied to the fields of flat panel display, solar cells, electrochromism and the like. Currently, an ITO thin film is mainly obtained by magnetron sputtering of an ITO target, and the quality of the ITO target determines the performance of the thin film.

Dry forming is a forming method commonly used for preparing an ITO target, and is mainly a forming process of mould pressing auxiliary isostatic pressing or direct isostatic pressing. The granulation technology is a core technology of dry molding, the prepared granulated powder has good mold filling property and fluidity and few defects, and in order to meet the requirement, the granulated powder is generally required to be solid and spherical, however, the ITO granulated powder prepared by the prior art is generally in a hollow apple shape, so that a high-quality target cannot be obtained.

The preparation of solid spherical granulation powder requires slurry with higher viscosity, but in order to ensure that the ITO powder is fully ground, a dispersant is usually added to reduce the viscosity of the slurry, so that in the actual production, the solid spherical granulation powder and the dispersant are difficult to be considered simultaneously to prepare the solid spherical granulation powder. The chinese patent publication No. CN106082993A discloses a method for producing solid spherical particles by granulating ITO powder, crushing, dispersing, and performing secondary granulation, but the process flow of the production method is complicated, and the production cost is increased substantially.

Therefore, it is necessary to find a method for manufacturing solid spherical ITO granulated powder with simple process and low cost.

Disclosure of Invention

In view of the above, the present invention aims to provide a preparation method of solid spherical ITO granulated powder, which can ensure sufficient grinding and dispersion of ITO granulated powder, can also prepare solid spherical ITO granulated powder, is convenient to operate, and meets the requirement of high performance target preparation.

The technical scheme adopted by the invention to solve the technical problems is as follows:

a preparation method of solid spherical ITO (indium tin oxide) granulation powder comprises the steps of mixing indium oxide powder, tin oxide powder and deionized water to prepare slurry, adding a dispersing agent into the slurry, fully grinding, adding a binder, uniformly mixing, heating the slurry or adjusting the pH value of the slurry to control the viscosity of the slurry to be 100-1500 mPa & s, and finally performing spray drying on the slurry to obtain the solid spherical ITO granulation powder.

Further, the specific operation of heating the slurry is as follows: and heating the slurry to 50-100 ℃, detecting the viscosity of the slurry in real time, and stopping heating when the viscosity of the slurry reaches the target viscosity.

Further, the specific operation of adjusting the pH of the slurry is: and adding any one of acetic acid, nitric acid or hydrochloric acid into the slurry to ensure that the pH of the slurry is less than 6.

Further, indium oxide powder with the particle size of 10-500 nm and tin oxide powder with the particle size of 10-500 nm are selected, and the indium oxide powder and the tin oxide powder are added into deionized water according to the mass ratio of 9:1 to prepare slurry with the solid content of 50-80%.

Further, the amount of the added dispersing agent is 0.1-5% of the total mass of the powder, and the dispersing agent is any one or the combination of more than two of polyacrylamide, polycarboxylic acid, polyacrylic acid, polyvinyl alcohol and polyethylene glycol.

Further, after the dispersing agent is added into the slurry and fully ground, the particle size of the slurry meets D90= 0.1-2 mu m.

Furthermore, the amount of the added binder is 1-10% of the total mass of the powder, and the binder is any one or the combination of more than two of polyvinyl alcohol, polyethylene glycol, polyacetal and polymethyl cellulose.

Further, during spray drying, the air inlet temperature is 100-300 ℃, the air outlet temperature is 60-200 ℃, and the frequency of the atomizer is 20-50 Hz.

Further, the particle size of the prepared ITO granulated powder is 20-150 mu m.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained based on these drawings without creative efforts.

FIG. 1 is a microstructure diagram of example 2 of the present invention.

Detailed Description

A preparation method of solid spherical ITO (indium tin oxide) granulation powder comprises the steps of selecting indium oxide powder with the particle size of 10-500 nm and tin oxide powder with the particle size of 10-500 nm, adding the indium oxide powder and the tin oxide powder into deionized water according to the mass ratio of 9:1, preparing slurry with the solid content of 50-80%, then adding a dispersing agent accounting for 0.1-5% of the total mass of the powder into the slurry, fully grinding the slurry, enabling the particle size of the ground slurry to meet D90= 0.1-2 mu m, then adding a binding agent accounting for 1-10% of the total mass of the powder into the slurry, and uniformly mixing the binder and the powder, and then heating the slurry or adjusting the pH value of the slurry to control the viscosity of the slurry to be 100-1500 mPa.s, finally performing spray drying on the slurry, and ensuring that the air inlet temperature is 100-300 ℃, the air outlet temperature is 60-200 ℃, and the frequency of an atomizer is 20-50 Hz, thus obtaining the solid spherical ITO granulated powder with the particle size of 20-150 mu m.

When the slurry is selected to be heated, the slurry is heated to 50-100 ℃, the viscosity of the slurry is detected in real time, and the heating can be stopped when the slurry reaches the target viscosity. . When the pH value of the slurry is selected to be adjusted, any one of acetic acid, nitric acid or hydrochloric acid is only required to be added into the slurry, so that the pH value of the slurry is less than 6.

Wherein the dispersant is any one or the combination of more than two of polyacrylamide, polycarboxylic acid, polyacrylic acid, polyvinyl alcohol and polyethylene glycol; the binder is any one or the combination of more than two of polyvinyl alcohol, polyethylene glycol, polyacetal and polymethyl cellulose.

It should be noted that the apparatus used in the following examples is an apparatus conventional in the art; experimental procedures in the following examples, where specific conditions are not noted, are generally carried out under conventional conditions, or under conditions recommended by the manufacturer; in the following examples, various starting materials were used, and unless otherwise specified, conventional commercially available products were used.