Method for preparing high-density rotating ITO target material from indium oxide with different specific surface areas

Abstract

The invention relates to the technical field of target materials, and provides a method for preparing a high-density rotating ITO target material from indium oxide with different specific surface areas, which comprises the following steps: mixing indium oxide powder with different specific surface areas to obtain tin oxide with the matching specific surface area of 10-12m < 2 > / g of 11.5 + / -1m < 2 > / g; the high-density ITO target material is obtained through powder mixing, slurry dispersion, slurry sanding, spray granulation, cold isostatic pressing forming, turning and sintering. The indium oxide powder of 11.5 + / -1m < 2 > / g is formed by mixing indium oxide powder of which the surface area is 6-10m < 2 > / g, indium oxide powder of which the specific surface area is 10-12.5 m < 2 > / g and indium oxide powder of which the specific surface area is 12.5-18m < 2 > / g for 500-1000 times, so that compared with direct use of the indium oxide powder of 11.5 + / -1m < 2 > / g, the ITO target material is prepared, and the target material with higher density can be obtained.

Description

Technical Field

[0001] The invention relates to the technical field of target materials, and in particular to a method for preparing a high-density rotating ITO target material from indium oxide with different specific surface areas. Background Art

[0002] ITO (IndiumTinOxide) refers to a compound target composed of three elements: indium, tin, and oxygen. Due to its excellent conductivity, transparency, and stability, it is widely used in the manufacture of flat-panel displays, solar panels, various optical glasses, and other optoelectronic fields. ITO targets are formed into transparent conductive electrodes through sputtering. With the rise of various mobile devices such as smartphones and tablets, as well as emerging fields such as smart homes and AI artificial intelligence, the demand for ITO targets is also increasing rapidly.

[0003] ITO targets will produce "poisoning" and particle and other abnormalities during the coating process, thus affecting the service life of the target and the quality of the ITO film. A large number of experiments have shown that increasing the density of the target can effectively improve such abnormalities; especially in ultra-low sputtering power environments, high-density targets can effectively reduce the abnormal discharge rate of the target and improve sputtering efficiency. At the same time, the increase in target density can improve the mechanical indicators such as target strength and hardness to a certain extent. The density of the target is closely related to the specific surface area of ​​indium oxide powder. Mixing indium oxide powders with different specific surface areas and then preparing ITO targets can improve the density of the target. Therefore, a method for preparing high-density rotating ITO targets with indium oxides of different specific surface areas is needed. Summary of the invention

[0004] In view of this, the purpose of the present invention is to propose a method for preparing a high-density rotating ITO target material using indium oxide with different specific surface areas, thereby solving the problems of the background technology.

[0005] Based on the above purpose, the present invention provides a method for preparing a high-density rotating ITO target material with indium oxide of different specific surface areas, comprising the following steps:

[0006] Step 1: Select indium oxide and tin oxide with a raw material powder purity of ≥99.99, and the specific surface area of ​​indium oxide is 11.5±1m 2 / g, tin oxide specific surface area 10-12m 2 / g, 11.5±1m 2 / g of indium oxide powder is prepared by mixing indium oxide powders with different specific surface areas;

[0007] Step 2, weighing raw material powders according to the weight ratio of indium oxide:tin oxide=90:10, mixing and blending, adding pure water at the same time, the weight of which is the same as the total weight of the powder, adding a dispersant, dispersing and stirring, and obtaining a slurry;

[0008] Step 3, transfer the dispersed slurry into a sand mill, use a grinding medium of 0.1-0.3mm, a rotation speed of 550-650 rpm, double-tank grinding, grinding 4-6 times, grinding time 6-8h, dispersant addition amount of 0.1-0.6%*total weight of powder, defoamer addition amount of 0.5-1.5%*total weight of powder, slurry water content of 35-40%, to obtain a final slurry particle size D50≤0.3um, D90≤0.75um;

[0009] Step 4: The qualified slurry is granulated into powder by a high-temperature spray granulator to obtain spherical powder that meets the standards;

[0010] Step 5: Add qualified powder into a special rotationally molded steel core and a polyurethane sheath, plug the two ends with plugs, and then hang it into a cold isostatic press for pressing to obtain a uniformly densified green embryo;

[0011] Step 6, turning the target blank after cold isostatic pressing to remove the two end corners;

[0012] Step seven, placing the turned target embryo into a normal pressure furnace for sintering, introducing oxygen during the sintering process, and finally obtaining a high-density rotating target material.

[0013] Preferably, the 11.5±1m 2 / g indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-95% specific surface area 10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed.

[0014] Preferably, the 11.5±1m 2 / g of indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-90% of which has a specific surface area of ​​10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed.

[0015] Preferably, in the step 1, the number of times of mixing indium oxide powders with different specific surface areas is 500-1000 times to obtain 11.5±1m 2 / g of indium oxide powder.

[0016] Preferably, in step 2, the stirring speed is 80-150 rpm and the stirring time is 3-5 h.

[0017] Preferably, in step 4, the air inlet temperature is 235±5°C and the air outlet temperature is 105±5°C.

[0018] Preferably, the molding pressure in step five is 300 MPa and the time is 2-3 hours.

[0019] Preferably, in step seven, the sintering temperature is 1500-1600° C., the time is 15-25 h, and the heating rate is 0.5-1.5° C. / min.

[0020] Beneficial effects of the present invention: The present invention obtains 11.5±1m by mixing indium oxide powders with different specific surface areas. 2 / g Mixed specific surface area 10-12m 2 / g of tin oxide, and a high-density ITO target is obtained by powder mixing, slurry dispersion, slurry sand grinding, spray granulation, cold isostatic pressing, turning, and sintering; the present invention 11.5±1m 2 / g indium oxide powder has a surface area of ​​6-10m 2 / g indium oxide powder 、 Specific surface area 10-12.5m 2 / g indium oxide powder, with a specific surface area of ​​12.5-18m 2 / g of indium oxide powder is mixed 500-1000 times to prepare ITO target. Compared with directly using 11.5±1m 2 / g of indium oxide powder can obtain a target with higher density. DETAILED DESCRIPTION

[0021] In order to make the objectives, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments.

[0022] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in the present invention should be understood by people with ordinary skills in the field to which the present invention belongs. The "first", "second" and similar words used in the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the described object changes, the relative positional relationship may also change accordingly.

[0023] Example 1

[0024] This embodiment provides a method for preparing a high-density rotating ITO target material using indium oxide with different specific surface areas, comprising the following steps:

[0025] S1, select indium oxide and tin oxide with a raw material powder purity of ≥99.99, and the specific surface area of ​​indium oxide is 11.5±1m 2 / g, tin oxide specific surface area 10-12m 2 / g;

[0026] S2, 11.5±1m 2 / g indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-95% specific surface area 10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed 500-1000 times.

[0027] S3, weighing raw material powders according to the weight ratio of indium oxide:tin oxide = 90:10, mixing and blending, adding pure water at the same weight as the total weight of the powder, adding a dispersant, and dispersing and stirring at a stirring speed of 80-150 rpm for 3-5 h to obtain a slurry;

[0028] S4, transfer the dispersed slurry into a sand mill, use a grinding medium of 0.1-0.3mm, a rotation speed of 550-650 rpm, use double tank grinding, grind 4-6 times, grind for 6-8h, add 0.1-0.6%*total weight of powder of dispersant, add 0.5-1.5%*total weight of powder of defoamer, and the water content of slurry is between 35-40%, and obtain the final slurry particle size D50≤0.3um, D90≤0.75um;

[0029] S5, the qualified slurry is granulated into powder by a high-temperature spray granulator, with an inlet temperature of 235±5℃ and an outlet temperature of 105±5℃, to obtain spherical powder that meets the standards;

[0030] S6, adding qualified powder into a special rotary forming steel core and polyurethane sheath, plugging both ends with plugs and hanging into a cold isostatic press for pressing, with a molding pressure of 300Mpa and a time of 2-3h to obtain a uniformly densified green embryo;

[0031] S7, turning the target blank after cold isostatic pressing to remove the two end corners;

[0032] S8, placing the turned target embryo into a normal pressure furnace for sintering, the sintering temperature is 1500-1600°C, the time is 15-25h, the heating rate is 0.5-1.5°C / min, oxygen is introduced during the sintering process, and finally a high-density rotating target material is obtained.

[0033] Example 2

[0034] This embodiment provides a method for preparing a high-density rotating ITO target material using indium oxide with different specific surface areas, comprising the following steps:

[0035] S1, select indium oxide and tin oxide with a raw material powder purity of ≥99.99, and the specific surface area of ​​indium oxide is 11.5±1m 2 / g, tin oxide specific surface area 10-12m 2 / g;

[0036] S2, 11.5±1m 2 / g of indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-90% of which has a specific surface area of ​​10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed 500-1000 times;

[0037] S3, weighing raw material powders according to the weight ratio of indium oxide:tin oxide = 90:10, mixing and blending, adding pure water at the same weight as the total weight of the powder, adding a dispersant, and dispersing and stirring at a stirring speed of 80-150 rpm for 3-5 h to obtain a slurry;

[0038] S4, transfer the dispersed slurry into a sand mill, use a grinding medium of 0.1-0.3mm, a rotation speed of 550-650 rpm, use double tank grinding, grind 4-6 times, grind for 6-8h, add 0.1-0.6%*total weight of powder of dispersant, add 0.5-1.5%*total weight of powder of defoamer, and the water content of slurry is between 35-40%, and obtain the final slurry particle size D50≤0.3um, D90≤0.75um;

[0039] S5, the qualified slurry is granulated into powder by a high-temperature spray granulator, with an inlet temperature of 235±5℃ and an outlet temperature of 105±5℃, to obtain spherical powder that meets the standards;

[0040] S6, adding qualified powder into a special rotary forming steel core and polyurethane sheath, plugging both ends with plugs and hanging into a cold isostatic press for pressing, with a molding pressure of 300Mpa and a time of 2-3h to obtain a uniformly densified green embryo;

[0041] S7, turning the target blank after cold isostatic pressing to remove the two end corners;

[0042] S8, placing the turned target embryo into a normal pressure furnace for sintering, the sintering temperature is 1500-1600°C, the time is 15-25h, the heating rate is 0.5-1.5°C / min, oxygen is introduced during the sintering process, and finally a high-density rotating target material is obtained.

[0043] Comparative Example

[0044] This embodiment provides a method for preparing a high-density rotating ITO target material using indium oxide with different specific surface areas, comprising the following steps:

[0045] S1, select indium oxide and tin oxide with a raw material powder purity of ≥99.99, and the specific surface area of ​​indium oxide is 11.5±1m 2 / g, tin oxide specific surface area 10-12m 2 / g;

[0046] S2, weighing raw material powders according to the weight ratio of indium oxide:tin oxide = 90:10, mixing and blending, adding pure water at the same weight as the total weight of the powder, adding a dispersant, and dispersing and stirring at a stirring speed of 80-150 rpm for 3-5 h to obtain a slurry;

[0047] S3, transfer the dispersed slurry into a sand mill, use a grinding medium of 0.1-0.3mm, a rotation speed of 550-650 rpm, double-tank grinding, grinding 4-6 times, grinding time 6-8h, dispersant addition amount of 0.1-0.6%*total weight of powder, defoamer addition amount of 0.5-1.5%*total weight of powder, slurry water content of 35-40%, to obtain the final slurry particle size D50≤0.3um, D90≤0.75um;

[0048] S4, the qualified slurry is passed through a high-temperature spray granulator for powder granulation, with an inlet temperature of 235±5°C and an outlet temperature of 105±5°C to obtain a spherical powder that meets the standards;

[0049] S5, adding qualified powder into a special rotary forming steel core and polyurethane sheath, plugging both ends with plugs and hanging into a cold isostatic press for pressing, with a molding pressure of 300Mpa and a time of 2-3h to obtain a uniformly densified green embryo;

[0050] S6, turning the target blank after cold isostatic pressing to remove the two end corners;

[0051] S7, placing the turned target embryo into a normal pressure furnace for sintering, the sintering temperature is 1500-1600°C, the time is 15-25h, the heating rate is 0.5-1.5°C / min, oxygen is introduced during the sintering process, and finally a high-density rotating target material is obtained.

[0052] The target properties obtained in Examples 1, 2 and Comparative Examples are shown in the following table:

[0053]

[0054] As can be seen from the above table, the present invention 11.5 ± 1m 2 / g indium oxide powder has a surface area of ​​6-10m 2 / g indium oxide powder 、 Specific surface area 10-12.5m 2 / g indium oxide powder, with a specific surface area of ​​12.5-18m 2 / g of indium oxide powder is mixed 500-1000 times to prepare ITO target. Compared with directly using 11.5±1m 2 / g of indium oxide powder can obtain a target with higher density.

[0055] It should be understood by those skilled in the art that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the present invention is limited to these examples; under the concept of the present invention, the technical features in the above embodiments or different embodiments may also be combined, the steps may be implemented in any order, and there are many other variations of the different aspects of the present invention as described above, which are not provided in detail for the sake of simplicity. Any omissions, modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of protection of the present invention.

Claims

1. A method for preparing high-density rotating ITO targets using indium oxides with different specific surface areas, characterized in that: The following steps are included: Step 1: Select indium oxide and tin oxide with a raw material powder purity of ≥99.99, and the specific surface area of ​​indium oxide is 11.5±1m 2 / g, tin oxide specific surface area 10-12m 2 / g, 11.5±1m 2 / g of indium oxide powder is prepared by mixing indium oxide powders with different specific surface areas; Step 2, weighing raw material powders according to the weight ratio of indium oxide:tin oxide=90:10, mixing and blending, adding pure water at the same time, the weight of which is the same as the total weight of the powder, adding a dispersant, dispersing and stirring, and obtaining a slurry; Step 3, transfer the dispersed slurry into a sand mill, use a grinding medium of 0.1-0.3mm, a rotation speed of 550-650 rpm, double-tank grinding, grinding 4-6 times, grinding time 6-8h, dispersant addition amount of 0.1-0.6%*total weight of powder, defoamer addition amount of 0.5-1.5%*total weight of powder, slurry water content of 35-40%, to obtain a final slurry particle size D50≤0.3um, D90≤0.75um; Step 4: The qualified slurry is granulated into powder by a high-temperature spray granulator to obtain spherical powder that meets the standards; Step 5: Add qualified powder into a special rotationally molded steel core and a polyurethane sheath, plug the two ends with plugs, and then hang it into a cold isostatic press for pressing to obtain a uniformly densified green embryo; Step 6, turning the target blank after cold isostatic pressing to remove the two end corners; Step seven, placing the turned target embryo into a normal pressure furnace for sintering, introducing oxygen during the sintering process, and finally obtaining a high-density rotating target material.

2. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: 11.5±1m 2 / g indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-95% specific surface area 10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed.

3. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: 11.5±1m 2 / g of indium oxide powder with a specific surface area of ​​6-10m 2 / g indium oxide powder, 80-90% of which has a specific surface area of ​​10-12.5m 2 / g indium oxide powder, ≤10% specific surface area 12.5-18m 2 / g of indium oxide powder is mixed.

4. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: In the step 1, the indium oxide powders with different specific surface areas are mixed 500-1000 times to obtain 11.5±1m 2 / g of indium oxide powder.

5. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: In step 2, the stirring speed is 80-150 rpm and the stirring time is 3-5 h.

6. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: In step 4, the air inlet temperature is 235±5°C and the air outlet temperature is 105±5°C.

7. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: The molding pressure in step 5 is 300 MPa and the time is 2-3 hours.

8. The method for preparing high-density rotating ITO target material using indium oxide with different specific surface areas according to claim 1, characterized in that: In step seven, the sintering temperature is 1500-1600° C., the time is 15-25 hours, and the heating rate is 0.5-1.5° C. / min.

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