Large-size AZO rotating target material with high compactness, low resistivity and few white skins and preparation method of large-size AZO rotating target material

The zinc oxide mixed powder is prepared by spray granulation and cold isostatic pressing technology and sintered in an inert atmosphere, which solves the problems of density and resistivity of AZO rotary targets in the prior art, and realizes the preparation of large-size AZO rotary targets with high density and low resistivity.

CN119735436AActive Publication Date: 2025-04-01LEADING THIN FILM MATERIALS (JIANGSU) CO LTD

Patent Information

Application Number
CN202411832879.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-13
Publication Date
2025-04-01
Estimated Expiration
2044-12-13

AI Technical Summary

Technical Problem

The existing zinc oxide aluminum target preparation method is difficult to prepare high-density, low resistivity and large-size AZO rotary targets, and there are problems of Zn element volatility and uneven surface components.

Method used

Spray granulation and cold isostatic pressing technology are used to prepare a mixed powder of zinc oxide and alumina. The temperature increase and cooling rate are controlled through inert atmosphere to ensure the high density and low resistivity of the target material.

Benefits of technology

The high density (relative density greater than 99.86%) and low resistivity (resistance less than 7-4Ωcm) of large-size AZO rotating targets are achieved, while reducing the formation of white skin to ensure good surface quality of the target.

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Abstract

The invention belongs to the technical field of target materials, and discloses a preparation method of a high-density, low-resistivity and few-white-skin large-size AZO rotating target material, which comprises the following steps: carrying out spray granulation on mixed slurry of zinc oxide and aluminum oxide to obtain mixed powder; filling the mixed powder into a mold, and carrying out cold isostatic pressing to obtain a green body; the isostatic cool pressing is performed in 4-6 sections, and the pressure of the latter section is 30-60 MPa higher than that of the former section; sintering the green body in an inert atmosphere, heating to 1300-1550 DEG C at a speed of 0.3-2 DEG C / min, preserving heat for 0.5-1 hour, then cooling to 1200-1350 DEG C at a speed of 2-5 DEG C / min, and preserving heat for 10-20 hours to obtain the AZO rotating target material. In an existing preparation technological process, a cold isostatic pressing mode, a sintering schedule and the like are changed, the rotating target material with the length larger than 500 mm, the outer diameter larger than 150 mm and the thickness larger than 20 mm can be obtained, the relative density of the rotating target material is larger than 99.86%, the electrical resistivity is lower than 7-4 ohm cm, the surface quality is good, white skin is few, the internal color and the external color are uniform, and the grain size is smaller than 15 micrometers.
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Description

Technical Field

[0001] The invention belongs to the technical field of target materials, and in particular relates to a method for preparing a zinc oxide aluminum target material. Background Art

[0002] With the application of semiconductor materials in scientific and technological fields such as computers and solar energy, the application fields of transparent conductive oxide films with superior optical and electrical properties have expanded from infrared radiation reflectors, energy-saving window glass, low-emissivity chain film glass, antistatic coatings and anti-icing and defrosting functional glass to optoelectronic fields such as modern liquid crystal displays, organic light-emitting diodes, flat panel displays, plasma displays, gas sensors and transparent electrodes. At present, the transparent conductive films prepared and produced industrially are mainly indium tin oxide (ITO) films, but the raw materials for its production are expensive and the cost is high; the visible light transmittance is low at high temperatures; and it is easily reduced in hydrogen ions, which affects the efficiency and life of solar cells. Aluminum-doped zinc oxide (AZO) film has abundant raw materials and low prices. The resistivity and average visible light transmittance can reach 10 respectively. -4 Ωcm and 85%; in addition, compared with ITO film, AZO film is more stable in hydrogen ion atmosphere and is a new type of transparent conductive oxide film.

[0003] CN115849896A discloses a zinc oxide target material and its preparation method and application. The zinc oxide powder is molded, cold isostatically pressed, degreased and sintered to obtain the zinc oxide target material; wherein the molding pressure of the zinc oxide blank is 200-400Mpa; the sintering temperature is 1000℃-1200℃. The preparation method of the zinc oxide target material of the invention is simple and low in cost, but the relative density of the target material can only reach 96%.

[0004] CN117756518A discloses a method for preparing a zinc oxide aluminum target material, wherein the zinc oxide aluminum target material is prepared by a spray drying and sintering process, static pressure molding, and sintering, wherein the molding pressure is 200 MPa, the sintering temperature is 1450°C, and the temperature is kept at 24 hours. The density of the zinc oxide aluminum target material is as high as 99%.

[0005] Under normal pressure sintering conditions, the density of the target tends to increase when the sintering temperature is increased appropriately. However, for AZO targets, high-temperature sintering causes the problem of Zn volatilization. Zinc oxide itself has the characteristics of a small amount of oxygen loss at 800°C and a small amount of volatilization at 1200°C. After a long period of high-temperature sintering, there will be an Al-rich area on the surface of the target, forming ZnAl2O4, which is a dielectric material and is not conductive. It will cause uneven surface components of the target, performance degradation, and increase the amount of post-processing.

[0006] In addition, the current preparation method of zinc oxide aluminum target (AZO target) is difficult to prepare qualified large-size AZO targets. Summary of the invention

[0007] In view of the problems existing in the prior art, the object of the present invention is to provide a method for preparing a large-size AZO rotating target material with high density, low resistivity and less white skin.

[0008] The large-size AZO rotary target described in the present invention refers to an AZO rotary target with a length greater than 500 mm, an outer diameter greater than 150 mm, and a thickness greater than 20 mm.

[0009] To achieve the above objectives, the present invention provides the following specific technical solutions.

[0010] A method for preparing a large-size AZO rotating target material with high density, low resistivity and less white skin, comprising: The mixed slurry of zinc oxide and aluminum oxide is sprayed and granulated to obtain a mixed powder; The mixed powder is molded and then cold isostatically pressed to obtain a green body; the cold isostatic pressing is performed in 4-6 stages, and during the pressurization process, the pressure of the latter stage is 30-60 MPa greater than the pressure of the former stage; The green body is sintered in an inert atmosphere, the temperature is increased to 1300°C~1550°C at a rate of 0.3°C / min~2°C / min and kept at that temperature for 0.5-1h, and then the temperature is decreased to 1200°C~1350°C at a rate of 2°C~5°C / min and kept at that temperature for 10-20h to obtain an AZO rotary target.

[0011] In a further preferred embodiment, the mass ratio of zinc oxide to aluminum oxide in the mixed slurry of zinc oxide and aluminum oxide is 99-98:1-2.

[0012] In a further preferred embodiment, the mixed slurry of zinc oxide and aluminum oxide is obtained by mixing zinc oxide slurry and aluminum oxide slurry.

[0013] Furthermore, a binder is added when the zinc oxide slurry and the aluminum oxide slurry are mixed.

[0014] Furthermore, the binder is at least one of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylic acid salt, and polyethylene glycol. Further preferably, the amount of the binder is 1-5% of the mass of the mixed slurry of zinc oxide and aluminum oxide.

[0015] Furthermore, the aluminum oxide powder, the first dispersant and water are mixed to form a slurry and ground to obtain an aluminum oxide slurry; the zinc oxide powder, the second dispersant and water are mixed to form a slurry and ground to obtain a zinc oxide slurry.

[0016] Furthermore, the first dispersant and the second dispersant are independently selected from one or more of polyvinyl pyrrolidone, sodium dodecylbenzene sulfonate, and sodium hexadecylbenzene sulfonate.

[0017] Furthermore, the amount of the first dispersant used is 1-5% of the mass of the aluminum oxide slurry; and the amount of the second dispersant used is 10-15% of the mass of the zinc oxide slurry.

[0018] In a further preferred embodiment, the spray granulation is carried out by a spray drying tower, the outlet air temperature of the spray drying tower is 130-200° C., and the atomizer frequency is 40-70 Hz.

[0019] In a further preferred embodiment, the bulk density of the mixed powder is 1.55-1.7 g / cm 3 .

[0020] In a further preferred embodiment, the cold isostatic pressing is carried out in 5 stages, the pressure of the first stage is 30-50 MPa, and the holding time is 3-6 min; the pressure of the second stage is 60-90 MPa, and the holding time is 2-6 min; the pressure of the third stage is 100-130 MPa, and the holding time is 1-3 min; the pressure of the fourth stage is 140-160 MPa, and the holding time is 1-3 min; the pressure of the fifth stage is 170~200 MPa, and the holding time is 10~15 min.

[0021] In a further preferred embodiment, the inert atmosphere is an argon atmosphere.

[0022] Based on the same inventive concept, the present invention provides a large-size rotating AZO target material, wherein the length of the large-size rotating AZO target material is greater than 500 mm, the outer diameter is greater than 150 mm, the thickness is greater than 20 mm, the relative density is greater than 99.86%, and the resistivity is less than 7 -4 Ωcm.

[0023] Further preferably, the grain size of the large-size rotating AZO target is less than 15 μm.

[0024] Compared with the prior art, the above one or more technical solutions of the present invention can achieve at least one of the following beneficial effects: The preparation method of the AZO rotary target provided by the present invention can prepare a rotary target with a length greater than 500 mm, an outer diameter greater than 150 mm, and a thickness greater than 20 mm, and the target has good surface quality, less white skin, uniform internal and external colors, and a grain size less than 15 μm.

[0025] In the existing preparation process, by changing the cold isostatic pressing method and sintering system, a relative density greater than 99.86% and a resistivity less than 7 -4The large-size AZO rotating target of Ωcm can utilize the existing production line without increasing the equipment and site costs.

[0026] The preparation method provided by the invention is simple and reliable. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 This is a SEM image of a cross section of the AZO rotary target obtained in Example 1. DETAILED DESCRIPTION

[0028] In order to facilitate the understanding of the present invention, the present invention will be described more comprehensively and meticulously below in conjunction with the accompanying drawings and preferred embodiments of the present invention, but the protection scope of the present invention is not limited to the following specific embodiments.

[0029] Unless otherwise defined, all the professional terms used below have the same meanings as those generally understood by those skilled in the art. The professional terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention.

[0030] Unless otherwise specified, various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or prepared by existing methods.

[0031] Example 1 Step 1: Weigh zinc oxide powder and aluminum oxide powder respectively according to the mass ratio of zinc oxide to aluminum oxide of 98:2 for later use.

[0032] Step 2: Add a certain amount of pure water and polyvinyl pyrrolidone dispersant into the dispersion tank, add the alumina powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 30 minutes, the dispersion speed is 180 rpm, and the amount of polyvinyl pyrrolidone accounts for 5% of the total mass of the material.

[0033] Step 3: The slurry obtained in step 2 was pumped into a sand mill by a pneumatic diaphragm pump for grinding for 6 hours at a grinding speed of 900 r / min to obtain alumina slurry.

[0034] Step 4: Add a certain amount of pure water and polyvinyl pyrrolidone dispersant into the dispersion tank, add the zinc oxide powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 40 minutes, the dispersion speed is 200 rpm, and the amount of polyvinyl pyrrolidone accounts for 15% of the total mass of the material.

[0035] Step 5: The slurry obtained in steps 3 and 4 is pumped into a sand mill with a pneumatic diaphragm pump and ground for 6 hours at a grinding speed of 800 r / min, and 1.8% polyvinyl alcohol of the mass of the slurry obtained in steps 3 and 4 is added to obtain a zinc oxide aluminum mixed slurry.

[0036] Step 6: The mixed slurry obtained in step 5 is fed into a spray drying tower for spray granulation, and then mixed and sieved to obtain a zinc oxide aluminum mixed powder. The air outlet temperature is 130°C, and the atomizer frequency is 70Hz. The powder bulk density is 1.7g / cm 3 .

[0037] Step 7: The mixed powder obtained in step 6 is molded into a rotating target (large size), and then cold isostatically pressed to obtain a zinc oxide aluminum target embryo. The process parameters of the cold isostatic pressing are: 30 MPa pressure maintenance for 3 minutes, 60 MPa pressure maintenance for 2 minutes, 90 MPa pressure maintenance for 1 minute, 120 MPa pressure maintenance for 3 minutes, and 180 MPa pressure maintenance for 15 minutes in the pressurization and pressure relief stages.

[0038] Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; first increase the temperature to 1550°C at a heating rate of 2°C / min and keep it for 0.5h, then cool it to 1350°C at a cooling rate of 4°C / min and keep it for 15h to obtain the target material.

[0039] Figure 1 This is a SEM image of a cross section of the AZO rotary target obtained in Example 1.

[0040] Comparative Example 1 The difference between Comparative Example 1 and Example 1 is that step 8 is different. Specifically: Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; increase the temperature to 1550°C at a heating rate of 2°C / min and keep it warm for 15 hours to obtain the target material.

[0041] Comparative Example 2 The difference between Comparative Example 2 and Example 1 is that step 7 is different. Specifically: Step 7: cold isostatically press the mixed powder obtained in step 6, increase the pressure to 180 MPa and maintain the pressure for 15 min.

[0042] Comparative Example 3 The difference between Comparative Example 3 and Example 1 is that step 7 is different. Specifically: Step 7: cold isostatic pressing the mixed powder obtained in step 6 to obtain a zinc oxide aluminum target embryo. The process parameters of the cold isostatic pressing are: 30 MPa pressure maintenance for 3 minutes, 50 MPa pressure maintenance for 2 minutes, 80 MPa pressure maintenance for 1 minute, 100 MPa pressure maintenance for 3 minutes, and 200 MPa pressure maintenance for 15 minutes in the pressurization and pressure relief stages.

[0043] Comparative Example 4 The only difference between Comparative Example 4 and Example 1 is that the heating rate in step 8 is 0.2° C. / min.

[0044] Comparative Example 5 The only difference between Comparative Example 5 and Example 1 is that the heating rate in step 8 is 2.5° C. / min.

[0045] Comparative Example 6 The only difference between Comparative Example 6 and Example 1 is that the cooling rate in step 8 is 1° C. / min.

[0046] Comparative Example 7 The only difference between Comparative Example 7 and Example 1 is that the cooling rate in step 8 is 6° C. / min.

[0047] Comparative Example 8 The only difference between Comparative Example 8 and Example 1 is that in step 8, the temperature is first increased to 1550°C at a heating rate of 2°C / min and kept at that temperature for 1.5 hours, and then the temperature is decreased to 1350°C at a cooling rate of 0.4°C / min and kept at that temperature for 15 hours.

[0048] Comparative Example 9 The difference between Comparative Example 9 and Example 1 is only that: Step 8 is different. Specifically: Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; increase the temperature to 1350°C at a heating rate of 2°C / min and keep it warm for 15 hours to obtain the target material.

[0049] Example 2 Step 1: Weigh zinc oxide powder and aluminum oxide powder respectively according to the mass ratio of zinc oxide to aluminum oxide of 98:2 for later use.

[0050] Step 2: Add a certain amount of pure water and sodium dodecylbenzene sulfonate dispersant into the dispersion tank, add the alumina powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 30 minutes, the dispersion speed is 180 rpm, and the amount of sodium dodecylbenzene sulfonate accounts for 3% of the total mass of the material.

[0051] Step 3: The slurry obtained in step 2 was pumped into a sand mill by a pneumatic diaphragm pump for grinding for 6 hours at a grinding speed of 900 r / min to obtain alumina slurry.

[0052] Step 4: Add a certain amount of pure water and sodium hexadecylbenzenesulfonate dispersant into the dispersion tank, add the zinc oxide powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 40 minutes, the dispersion speed is 200 rpm, and the amount of sodium hexadecylbenzenesulfonate accounts for 12% of the total mass of the material.

[0053] Step 5: The slurry obtained in steps 3 and 4 is pumped into a sand mill with a pneumatic diaphragm pump and ground for 6 hours at a grinding speed of 800 r / min, and 5% polyacrylamide of the mass of the slurry obtained in steps 3 and 4 is added to obtain a zinc oxide aluminum mixed slurry.

[0054] Step 6: The mixed slurry obtained in step 5 is fed into a spray drying tower for spray granulation, and then mixed and sieved to obtain a zinc oxide aluminum mixed powder. The air outlet temperature is 150°C, and the atomizer frequency is 50Hz. The bulk density of the mixed powder is 1.7g / cm 3 .

[0055] Step 7: The mixed powder obtained in step 6 is molded into a rotating target (large size), and then cold isostatically pressed to obtain a zinc oxide aluminum target embryo. The process parameters of the cold isostatic pressing are: 40Mpa pressure maintenance for 5 minutes, 70Mpa pressure maintenance for 2 minutes, 120Mpa pressure maintenance for 2 minutes, 150Mpa pressure maintenance for 2 minutes, and 200Mpa pressure maintenance for 10 minutes in the pressurization and pressure relief stages.

[0056] Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; first increase the temperature to 1450°C at a heating rate of 1°C / min and keep it for 1h, then cool it to 1300°C at a cooling rate of 2°C / min and keep it for 20h to obtain the target material.

[0057] Example 3 Step 1: Weigh zinc oxide powder and aluminum oxide powder respectively according to the mass ratio of zinc oxide to aluminum oxide of 99:1 for later use.

[0058] Step 2: Add a certain amount of pure water and sodium dodecylbenzene sulfonate dispersant into the dispersion tank, add the alumina powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 30 minutes, the dispersion speed is 180 rpm, and the amount of polyvinyl pyrrolidone accounts for 1% of the total mass of the material.

[0059] Step 3: The slurry obtained in step 2 was pumped into a sand mill by a pneumatic diaphragm pump for grinding for 6 hours at a grinding speed of 900 r / min to obtain alumina slurry.

[0060] Step 4: Add a certain amount of pure water and sodium hexadecylbenzene cyclopentane dispersant into the dispersion tank, add the zinc oxide powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 40 minutes, the dispersion speed is 200 rpm, and the amount of polyvinyl pyrrolidone accounts for 10% of the total mass of the material.

[0061] Step 5: The slurry obtained in steps 3 and 4 is pumped into a sand mill with a pneumatic diaphragm pump and ground for 6 hours at a grinding speed of 800 r / min, and 1% carboxymethyl cellulose is added based on the mass of the slurry obtained in steps 3 and 4 to obtain a zinc oxide aluminum mixed slurry.

[0062] Step 6: The mixed slurry obtained in step 5 is fed into a spray drying tower for spray granulation, and then mixed and sieved to obtain a zinc oxide aluminum mixed powder. The air outlet temperature is 200°C, and the atomizer frequency is 60Hz. The powder bulk density is 1.65g / cm 3 .

[0063] Step 7: The mixed powder obtained in step 6 is molded into a rotating target (large size), and then cold isostatically pressed to obtain a zinc oxide aluminum target embryo. The process parameters of the cold isostatic pressing are: 50 MPa pressure maintenance for 3 minutes, 90 MPa pressure maintenance for 2 minutes, 120 MPa pressure maintenance for 2 minutes, 150 MPa pressure maintenance for 2 minutes, and 180 MPa pressure maintenance for 10 minutes in the pressurization and pressure relief stages.

[0064] Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; first increase the temperature to 1300°C at a heating rate of 0.5°C / min and keep it for 0.5h, then cool it to 1200°C at a cooling rate of 5°C / min and keep it for 20h to obtain the target material.

[0065] Example 4 Step 1: Weigh zinc oxide powder and aluminum oxide powder respectively according to the mass ratio of zinc oxide to aluminum oxide of 99:1 for later use.

[0066] Step 2: Add a certain amount of pure water and polyvinyl pyrrolidone dispersant into the dispersion tank, add the alumina powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 30 minutes, the dispersion speed is 180 rpm, and the amount of polyvinyl pyrrolidone accounts for 2% of the total mass of the material.

[0067] Step 3: The slurry obtained in step 2 was pumped into a sand mill by a pneumatic diaphragm pump for grinding for 6 hours at a grinding speed of 900 r / min to obtain alumina slurry.

[0068] Step 4: Add a certain amount of pure water and polyvinyl pyrrolidone dispersant into the dispersion tank, add the zinc oxide powder weighed in step 1 into the dispersion tank for pre-dispersion, the dispersion time is 40 minutes, the dispersion speed is 200 rpm, and the amount of polyvinyl pyrrolidone accounts for 12% of the total mass of the material.

[0069] Step 5: The slurry obtained in steps 3 and 4 is pumped into a sand mill with a pneumatic diaphragm pump and ground for 6 hours at a grinding speed of 800 r / min, and 3% polyvinyl alcohol is added based on the mass of the slurry obtained in steps 3 and 4 to obtain a zinc oxide aluminum mixed slurry.

[0070] Step 6: The mixed slurry obtained in step 5 is fed into a spray drying tower for spray granulation, and then mixed and sieved to obtain zinc oxide aluminum mixed powder. The air outlet temperature is 180°C, and the atomizer frequency is 40Hz. The bulk density of the mixed powder is 1.7g / cm 3 .

[0071] Step 7: The mixed powder obtained in step 6 is molded into a rotating target (large size), and then cold isostatically pressed to obtain a zinc oxide aluminum target embryo. The process parameters of the cold isostatic pressing are: 50 MPa pressure maintenance for 3 minutes, 90 MPa pressure maintenance for 2 minutes, 130 MPa pressure maintenance for 2 minutes, 170 MPa pressure maintenance for 3 minutes, and 200 MPa pressure maintenance for 15 minutes in the pressurization and pressure relief stages.

[0072] Step 8: Sinter the zinc oxide aluminum target embryo, introduce argon gas into the sintering furnace to exhaust the air, and continue to introduce argon gas at a rate of 40L / min, and maintain the temperature of the argon gas to ensure stable heating and cooling during the sintering process; first increase the temperature to 1350°C at a heating rate of 0.3°C / min and keep it for 1h, then cool it to 1200°C at a cooling rate of 3°C / min and keep it for 20h to obtain the target material.

[0073] The relative density, resistivity, white skin thickness and grain size of AZO target were tested in the following ways.

[0074] (1) Relative density: Archimedes drainage method.

[0075] (2) Resistivity: four-probe method.

[0076] (3) White cortex thickness: measured with a vernier caliper.

[0077] (4) Grain size: determined by measuring the grain size in the SEM image.

[0078] The results are shown in Table 1.

[0079] Table 1 From the data in Table 1, it can be seen that in order to obtain a large-sized AZO rotating target material with high relative density, low resistivity and less white skin, the cold isostatic pressing and sintering system are very critical in the preparation process. The heating or cooling rate is low, and the surface of the obtained rotating target material has more white skin; the high-temperature insulation time is long, the white skin increases, and the grain size increases. The target material prepared by the preparation method of the large-sized AZO rotating target material provided by the present invention has good surface quality, less white skin, uniform color inside and outside, grain size less than 15μm, relative density greater than 99.86%, resistivity less than 7 -4 Ωcm.

[0080] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a large-size AZO rotating target with high density, low resistivity and less white skin, characterized in that: include: The mixed slurry of zinc oxide and aluminum oxide is sprayed and granulated to obtain a mixed powder; The mixed powder is molded and then cold isostatically pressed to obtain a green body; the cold isostatic pressing is performed in 4 to 6 stages, and during the pressurization process, the pressure of the latter stage is 30 to 60 MPa greater than the pressure of the former stage; The green body is sintered in an inert atmosphere, the temperature is increased to 1300°C~1550°C at a rate of 0.3°C / min~2°C / min and kept at this temperature for 0.5~1h, and then the temperature is decreased to 1200°C~1350°C at a rate of 2°C~5°C / min and kept at this temperature for 10~20h to obtain an AZO rotary target.

2. The preparation method according to claim 1, characterized in that The mass ratio of zinc oxide to aluminum oxide in the mixed slurry of zinc oxide and aluminum oxide is 99-98:1-2.

3. The preparation method according to claim 1 or 2, characterized in that: The mixed slurry of zinc oxide and aluminum oxide is obtained by mixing zinc oxide slurry and aluminum oxide slurry; Mixing aluminum oxide powder, a first dispersant, and water to prepare a slurry and grinding to obtain an aluminum oxide slurry; The zinc oxide powder, the second dispersant and water are mixed to prepare a slurry and then ground to obtain a zinc oxide slurry.

4. The preparation method according to claim 3, characterized in that: When mixing zinc oxide slurry and aluminum oxide slurry, a binder is added; the binder is at least one of polyvinyl alcohol, carboxymethyl cellulose, polyacrylamide, polyacrylic acid salt, and polyethylene glycol; the amount of the binder is 1-5% of the mass of the mixed slurry of zinc oxide and aluminum oxide.

5. The preparation method according to claim 3, characterized in that: The first dispersant and the second dispersant are independently selected from one or more of polyvinyl pyrrolidone, sodium dodecylbenzene sulfonate, and sodium hexadecylbenzene sulfonate; the amount of the first dispersant is 1-5% of the mass of the alumina slurry; the amount of the second dispersant is 10-15% of the mass of the zinc oxide slurry.

6. The preparation method according to claim 1, characterized in that: The spray granulation is carried out by a spray drying tower, wherein the outlet air temperature of the spray drying tower is 130-200° C. and the atomizer frequency is 40-70 Hz.

7. The preparation method according to claim 1, characterized in that: The cold isostatic pressing is carried out in 5 stages, the pressure of the first stage is 30-50 MPa, and the holding time is 3-6 min; the pressure of the second stage is 60-90 MPa, and the holding time is 2-6 min; the pressure of the third stage is 100-130 MPa, and the holding time is 1-3 min; the pressure of the fourth stage is 140-160 MPa, and the holding time is 1-3 min; the pressure of the fifth stage is 170-200 MPa, and the holding time is 10-15 min.

8. The preparation method according to claim 1, characterized in that: The inert atmosphere is an argon atmosphere.

9. A large-size rotating AZO target, characterized in that: The large-size rotating AZO target has a length greater than 500 mm, an outer diameter greater than 150 mm, a thickness greater than 20 mm, a relative density greater than 99.86%, and a resistivity less than 7 -4 Ωcm.

10. The large-size rotating AZO target according to claim 9, characterized in that: The grain size of the large-size rotating AZO target is less than 15 μm.

Citation Information

Patent Citations

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