Preparation method of aluminum zinc oxide AZO alloy target material

Through the vacuum rolling mixer mixer mixer mixing and vacuum hot press sintering process, the problems of cracking and low density during the molding of zinc-aluminum AZO alloy targets are solved, and uniform shrinkage and excellent performance of high-hardness and high resistance targets are achieved, reducing production costs.

CN120192159APending Publication Date: 2025-06-24HUNAN YUFENG VACUUM SCI & TECH CO LTD
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Patent Information

Application Number
CN202510349083.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-24
Publication Date
2025-06-24

AI Technical Summary

Technical Problem

Zinc-aluminum AZO alloy targets are prone to cracking and low density problems during the molding process, and the shrinkage of high-hardness and high resistance targets is difficult to control evenly during the sintering process.

Method used

The vacuum rolling mixer is used to mix zinc oxide and alumina, and the density and structure of the target material are controlled through vacuum hot pressing and rotary target material production process to ensure uniformity and high-quality finished products.

Benefits of technology

It effectively solves the problems of cracking and low density during the target forming process, achieves uniform shrinkage and excellent performance of high-hardness and high resistance targets, and reduces production costs.

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Abstract

The invention provides a preparation method of an aluminum zinc oxide AZO alloy target material, and belongs to the technical field of alloy target materials. The preparation method comprises the following steps: mixing zinc oxide and aluminum oxide in a vacuum rolling mixer, carrying out plasma spraying on the obtained mixture, placing the obtained mixture in a target material cavity, carrying out vacuum pumping treatment, introducing inert gas into the target material cavity, and mixing zinc oxide and aluminum oxide in the vacuum rolling mixer under the atmosphere condition of the inert gas, and the obtained AZO spraying powder is cold-sprayed to a cylinder of the target material, the spraying thickness of each time is 0.1 mm, the optimal rotating target material is prepared through repeated spraying, and the rotating target finished product is obtained after machining. Due to the fact that the rotating target material can rotate by 360 degrees in the coating process, the cylindrical rotating target can be evenly etched by 360 degrees, and the utilization rate of the target material can reach 90% at a time. The production cost of a planar target and a rotary target material is greatly reduced, and the prepared target material has the excellent properties of uniform structure, fine crystal grains, high thermal shock resistance and the like, so that the method is suitable for producing a large-area high-hardness high-resistance thin film.
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Description

Technical Field

[0001] This application belongs to the technical field of alloy targets, and particularly relates to a preparation method of aluminum-doped zinc oxide (AZO) alloy targets. Background Art

[0002] Chemically mixed AZO is the abbreviation of aluminum-doped zinc oxide (ZnO) transparent conductive glass. ZnO is rich in sources, inexpensive, non-toxic, and has excellent comprehensive properties. It has become a research hotspot of semiconductor optoelectronic materials internationally. ZnO thin film is an important optoelectronic information material. It not only has comparable optoelectronic properties to traditional ITO thin films, but also has rich raw materials, low price, non-toxicity, and high thermal stability. It has broad application prospects in the fields of solar cells, liquid crystal displays, and photodetectors. It can be widely used in the manufacture of flexible substrate light-emitting devices, plastic liquid crystal displays, and amorphous silicon solar cells. It can also be used as a transparent heat-insulating material for plastic greenhouses and the film coating of automotive glass and civil building glass. Especially in the ITO transparent conductive thin film of the optoelectronic industry, the In element is scarce and expensive. There is an urgent need to find a substitute material.

[0003] Doping Al in the ZnO system to obtain ZnO:Al transparent conductive thin film, that is, AZO thin film. After doping, the conductivity of the thin film is greatly improved. Moreover, the stability of the transparent conductive thin film AZO thin film in hydrogen plasma is better than that of ITO. At the same time, it has comparable optoelectronic characteristics to ITO. In addition, the preparation of AZO thin film is convenient, the elemental resources are richer than In element, and it is non-toxic. It has gradually become the best substitute for ITO thin film. AZO thin film has been partially applied in flat panel displays and thin film solar cells.

[0004] There are many methods for preparing AZO thin films, mainly including magnetron sputtering method, metal organic chemical vapor deposition method, pulsed laser deposition method, spray pyrolysis method, molecular beam epitaxy method, and sol-gel method, etc. Among them, the magnetron sputtering method for preparing AZO thin films has the advantages of high deposition rate, low substrate temperature, and good substrate adhesion, and is widely used.

[0005] In the preparation method of magnetron sputtered AZO film, the most widely studied and applied is the magnetron sputtering technology. The magnetron sputtering technology began to be applied in practice in the 1970s. The principle of preparing thin films is as follows: While filling an inert gas (Ar) with a pressure of 0.1 - 10 Pa into the vacuum chamber, a strong magnet of 100 - 1600 Gauss is placed under the cathode target. Under the action of high voltage, electrons collide with argon atoms during the process of accelerating towards the substrate under the action of the electric field, ionizing a large number of argon ions and electrons, and the electrons fly towards the substrate. The argon ions are accelerated under the action of the electric field to bombard the target, sputtering a large number of target atoms, and the neutral target atoms (or molecules) are deposited on the substrate to form a film. Secondary electrons are affected by the magnetic Lorentz force during the process of accelerating towards the substrate and are confined in the plasma region near the target surface. The plasma density in this region is very high. The secondary electrons move in a circular motion around the target surface under the action of the magnetic field. The movement path of this electron is very long, and it continuously collides with argon atoms during the movement process, ionizing a large number of argon ions to bombard the target. After multiple collisions, the energy of the electrons gradually decreases, breaks away from the restraint of the magnetic field lines, moves away from the target, and finally is deposited on the substrate. It has the advantages of high deposition rate, low substrate deposition temperature, good film adhesion, easy control, low cost, and can realize large-area film preparation. The AZO thin film with high hardness and high resistance has the advantages of anti-static, anti-radiation, anti-magnetic interference, high brightness, and high contrast. However, cracking and low density problems are likely to occur during the process of controlling the forming of the target, and it is difficult to uniformly control the shrinkage of the high-hardness and high-resistance target during the sintering process. The most difficult-to-control links in the existing casting technology mainly include the following: First, the quantitative control of gases, trace impurities, and inclusions in the melt; second, the control of shrinkage porosity, cracks, and uneven structure in large-sized ingots; third, problems such as surface pores, inclusions, and chemical waste products are also difficult to control. Summary of the Invention

[0006] The present application provides a preparation method of zinc oxide aluminum AZO alloy target, aiming to solve to a certain extent the problems of cracking and low density that are likely to occur during the process of controlling the forming of the target, and the problem that it is difficult to uniformly control the shrinkage of the high-hardness and high-resistance target during the sintering process.

[0007] In the first aspect, the present application provides a preparation method of zinc oxide aluminum AZO alloy target, including the following steps:

[0008] S1. Place zinc oxide and aluminum oxide in a vacuum rolling mixer for mixing to obtain a mixture;

[0009] S2. Select several points arbitrarily in the mixed material to detect the contents of zinc oxide and aluminum oxide until the mean error of the ratio of the zinc oxide content and the aluminum oxide content at each detection point is lower than the error set value;

[0010] S3. Fill the mixed material after being detected in S2 into a mold for pre-pressing to obtain a green blank, and then perform secondary pressing on the green blank to obtain a green body of an aluminum zinc oxide AZO alloy target.

[0011] S4. Production of planar target: Vacuum hot press and sinter the green body of the aluminum zinc oxide AZO alloy target, demold and cool it to obtain a rough product of the aluminum zinc oxide AZO alloy target; machine the rough product of the aluminum zinc oxide AZO alloy target to the required size, and anneal and clean it to obtain a planar target of the aluminum zinc oxide AZO alloy target.

[0012] S5. Production of rotary target: Ball mill and screen the mixed material after being detected in S2 to obtain aluminum zinc oxide spraying powder, take the cylinder of the green body of the aluminum zinc oxide AZO alloy target obtained in step S3, and cold spray it onto the cylinder target. The spraying thickness each time is 0.1 mm, and it is sprayed multiple times to obtain a superior rotary target, and after processing, a rotary target of the aluminum zinc oxide AZO alloy target is obtained.

[0013] In some embodiments, in S1, the mass ratio of zinc oxide to aluminum oxide is (5 - 9):(1 - 5), the Fisher average particle size of zinc oxide is 1 - 7 μm, and the Fisher average particle size of aluminum oxide is 1 - 7 μm.

[0014] In some embodiments, it is characterized in that in S1, in the vacuum rolling mixer, the pressure is 2 Pa and the rotation speed is 50 - 80 r / min for mixing.

[0015] In some embodiments, the error set value in S2 is less than 0.03%.

[0016] In some embodiments, the pressure of the pre-pressing in S3 is 10 - 60 MPa, the pressure of the secondary pressing is 50 - 200 MPa, and the density of the green body of the alloy target is 60 - 62% of the theoretical density.

[0017] In some embodiments, the vacuum hot press sintering in S4 is carried out under an argon protection atmosphere, the pressure is 20 - 30 MPa, the temperature is 1800 - 2000 °C, and heat preservation and pressure holding are carried out for 3 - 4 hours; the demolding is carried out under the condition of 500 - 600 °C.

[0018] 7 In some embodiments, the conditions for annealing in S4 are: in a vacuum annealing furnace, heat up to 1800 - 1980 °C and anneal for 3 - 4 h.

[0019] In some embodiments, in S5, ball milling is carried out for 3 - 5 h, and screening through a 1000 - mesh sieve to obtain AZO spraying powder.

[0020] Compared with the prior art, the beneficial effects of this application are:

[0021] 1. The production process technology of this solution is to mix zinc oxide and aluminum oxide in a vacuum rolling mixer to obtain a mixture, perform plasma spraying on the mixture, place the obtained mixture in a target chamber for vacuum treatment, then introduce an inert gas into it, and under the atmosphere condition of the inert gas, mix zinc oxide and aluminum oxide in a vacuum rolling mixer. Cold-spray the obtained AZO spraying powder onto the cylinder of the target, with each spraying thickness being 0.1 mm, and repeatedly spray to produce a high-quality rotating target, and obtain a finished rotating target after processing. Since the rotating target can rotate 360° during the film coating process, the cylinder rotating target is uniformly etched after rotating 360°, and the target material utilization rate can reach 90% at one time. This greatly reduces the production costs of planar targets and rotating targets, and the prepared target has excellent properties such as uniform structure, fine grains, and high heat shock resistance, thus being suitable for the production of large-area, high-hardness, and high-resistance films. Detailed implementation manners

[0022] In order to make the technical problems, technical solutions, and beneficial effects to be solved by this application clearer and more understandable, the following further elaborates on this application in combination with embodiments. It should be understood that the specific embodiments described herein are only used to explain this application and are not used to limit this application.

[0023] In this application, the term "and / or" describes the association relationship of associated objects, indicating that three relationships can exist. For example, A and / or B can represent: A exists alone, A and B exist simultaneously, and B exists alone. Where A and B can be singular or plural. The character " / " generally represents an "or" relationship between the associated objects before and after.

[0024] In this application, "at least one" means one or more, and "a plurality" means two or more. "At least one (item)" or its similar expression below refers to any combination of these items, including any combination of single item (item) or plural items (items). For example, "at least one (item) of a, b, or c", or, "at least one (item) of a, b, and c" can both represent: a, b, c, a to b (that is, a and b), a to c, b to c, or a to b to c, where a, b, and c can be single or multiple respectively.

[0025] The terms "first" and "second" are only used for descriptive purposes to distinguish objects such as substances from each other, and cannot be understood as indicating or implying relative importance or implicitly indicating the quantity of the indicated technical features. For example, without departing from the scope of the implementation regulations of this application, the first XX can also be called the second XX, and similarly, the second XX can also be called the first XX. Thus, the features defined with "first" and "second" can explicitly or implicitly include one or more of such features.

[0026] The terms used in the embodiments of the present application are for the purpose of describing specific embodiments only and are not intended to limit the present application. The singular forms "a", "the" and "said" used in the embodiments of the present application and the appended claims are also intended to include the plural forms unless the context clearly indicates otherwise.

[0027] It should be understood that in various embodiments of the present application, the magnitude of the serial numbers of the various processes does not mean the order of execution. Some or all of the steps may be executed in parallel or sequentially. The execution order of the various processes should be determined by their functions and internal logics and should not constitute any limitation to the implementation process of the embodiments of the present application.

[0028] The weights of the relevant components mentioned in the specification of the embodiments of the present application may not only refer to the specific contents of the various components, but also represent the proportional relationship of the weights between the various components. Therefore, as long as the contents of the relevant components in the specification of the embodiments of the present application are enlarged or reduced in proportion, they are within the scope disclosed in the specification of the embodiments of the present application. Specifically, the mass described in the specification of the embodiments of the present application may be mass units well-known in the chemical industry such as μg, mg, g, kg, etc.

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

[0030] Unless otherwise specifically stated, various raw materials, reagents, instruments and equipment used in the present application can be obtained through market purchase or can be prepared by existing methods.

[0031] The technical solutions of the present application will be described below through specific examples and comparative examples.

[0032] To enable those skilled in the art to clearly understand the above-mentioned implementation details and operations of the present application, and to significantly reflect the progressive performance of the embodiments of the present application, the above-mentioned technical solutions will be illustrated by multiple examples below.

[0033] Example 1:

[0034] A method for preparing an aluminum zinc oxide (AZO) alloy target:

[0035] S1. The furnace capacity of the vacuum rolling mixer is 30.0 kg. Zinc oxide powder with a theoretical density above 98% and a Fisher average particle size of 7 μm, and alumina powder with a theoretical density above 99.9% and a Fisher average particle size of 1 - 7 μm are respectively selected. 24.00 kg of zinc oxide and 6.00 kg of alumina are weighed according to the mass ratio of zinc oxide to alumina of 8:2, and are put into a vacuum pressure rolling mixer at 2×10° Pa, and are fully mixed under the condition of a rotation speed of 70 r / min;

[0036] S2. Arbitrarily select five points in the material mixed in step S1 to detect the zinc oxide content and alumina content until the error ratio of the zinc oxide content and alumina content at each detection point is within 0.01%, and the mixing is completed;

[0037] S3. Fill the mixed material processed in step S2 into a rubber sleeve equipped with a tubular flexible mold, and apply indium disulfide powder on the contact surface between the mold and the mixed material. Then seal the rubber sleeve and evacuate it, and place the evacuated rubber sleeve on a cold isostatic press, and perform primary pre-pressing under the condition of a pressure of 40 MPa to form a rough blank. The obtained rough blank is subjected to secondary pressing under the condition of 100 MPa until the density of the green compact reaches 60% of the theoretical density, and the pressure is released to normal pressure;

[0038] S4. Place the green compact of the zinc-aluminum alloy target pressed in step S3 into a vacuum hot pressing sintering furnace, and perform hot pressing sintering under the conditions of an argon protection atmosphere, a pressure of 20 MPa, and a temperature of 1900 °C. After heat preservation and pressure holding for 3 hours, use a high-temperature demolding process to demold at 500 °C, and cool to room temperature to obtain a rough product of the zinc oxide-aluminum alloy target; machine it to the required size, and then place it in a vacuum annealing furnace, heat up to 1800 °C and anneal for 3 hours; perform chemical and physical inspections on the obtained rough product of the zinc oxide-aluminum alloy target, and then perform ultrasonic cleaning to make the roughness of the target meet the requirements, and then obtain the finished product of the zinc oxide-aluminum alloy planar target after processing and cleaning;

[0039] S5. Rotating target production: Take the mixed material processed in step S2, and put the mixed material into a ball mill and ball mill for 3 hours, and pass through a 1000-mesh sieve to obtain zinc oxide-aluminum spraying powder;

[0040] Under the protection atmosphere of inert gas, use the plasma spraying method to spray the obtained zinc oxide-aluminum spraying powder on the outer surface of the finished product of the zinc oxide-aluminum alloy planar target in step S4 to obtain the target cavity;

[0041] The obtained target chamber is evacuated, and then an inert gas is introduced into it. The gas flow rate is 1200 sccm. Under the atmosphere of the inert gas, the aluminum zinc oxide spray powder is cold-sprayed into the inner cylindrical tube of the target chamber. The spraying thickness each time is 0.1 mm, and the total thickness reaches 11 mm. Through this process, a primary product of the (8:2) AZO alloy cylindrical target is obtained. After processing and cleaning, the finished product of the aluminum zinc oxide alloy cylindrical target is obtained.

[0042] Using the above-prepared aluminum zinc oxide alloy target as a rotating target, the Ar flow rate in the coating chamber is 200 sccm, the oxygen flow rate is 0.5 sccm, the vacuum degree of the coating chamber is between 3.0×10 -1 Pa, the total gas pressure is 0.30 Pa, the coating temperature is 350 °C. After coating, the thickness of the obtained film is 1.3 nm, and the resistance of the obtained coated product is 6×10 7 ohm, and the transmittance > 96%.

[0043] Example 2:

[0044] A preparation method of an aluminum zinc oxide AZO alloy target:

[0045] S1. The furnace capacity of the vacuum rolling mixer is 30.0 kg; zinc oxide powder with a theoretical density above 98% and a Fisher average particle size of 7 μm and aluminum oxide powder with a theoretical density above 99.9% and a Fisher average particle size of 7 μm are respectively selected. 21.00 kg of zinc oxide and 9.00 kg of aluminum oxide are weighed according to the mass ratio of zinc oxide to aluminum oxide of 7:3, and are put into a vacuum pressure rolling mixer at 2 Pa according to the mass ratio. Under the condition of a rotation speed of 50 r / minr / min, they are fully mixed;

[0046] S2. Five points are randomly selected from the materials mixed in step S1 to detect the indium oxide content and aluminum oxide content until the error of the zinc oxide content and aluminum oxide content ratio at each detection point is within 0.02%, and the mixing is completed;

[0047] S3. The mixed materials processed in step S2 are filled into a rubber sleeve equipped with a tubular flexible mold, and indium disulfide powder is smeared on the contact surface between the mold and the mixed materials. Then the rubber sleeve is sealed and evacuated, and the evacuated rubber sleeve is placed on a cold isostatic press. Under the condition of a pressure of 40 MPa, primary pre-pressing is carried out to form a rough blank. The obtained rough blank is subjected to secondary pressing under the condition of 100 MPa until the density of the green body reaches 60% of the theoretical density, and the pressure is released to normal pressure;

[0048] S4. Place the green body of the zinc-aluminum alloy target pressed in step S3 into a vacuum hot-pressing sintering furnace, and conduct hot-pressing sintering under the protection of argon atmosphere, at a pressure of 25 MPa and a temperature of 1900 °C. After heat preservation and pressure holding for 3 hours, use a high-temperature demolding process to demold at 500 °C, and cool to room temperature to obtain a rough zinc-aluminum oxide alloy target. Machine it to the required size, then place it in a vacuum annealing furnace, heat up to 1800 °C and anneal for 3 hours; conduct chemical and physical tests on the obtained rough zinc-aluminum oxide alloy target, and after ultrasonic cleaning, make the roughness of the target meet the requirements, and then obtain the finished zinc-aluminum oxide alloy planar target after processing and cleaning;

[0049] S5. Production of rotary target: Take the mixed material treated in step S2, and put the mixed material into a ball mill for ball milling for 3 hours, and pass through a 1000-mesh sieve to obtain zinc-aluminum oxide spraying powder;

[0050] Under the protection of an inert gas atmosphere, use the plasma spraying method to spray the obtained zinc-aluminum oxide spraying powder on the outer surface of the finished zinc-aluminum oxide alloy planar target in step S4 to obtain the target cavity;

[0051] The obtained target cavity is subjected to vacuum treatment, and then an inert gas is introduced into it, with a gas flow rate of 1200 sccm, and the zinc-aluminum oxide spraying powder is cold-sprayed into the inner cylindrical tube of the target cavity under the atmosphere condition of the inert gas. The thickness of each spraying is 0.1 mm, and the total thickness reaches 11 mm. After that, the initial product of the (7:3) AZO alloy cylindrical target is obtained, and then the finished zinc-aluminum oxide alloy cylindrical target is obtained after processing and cleaning.

[0052] Using the zinc-aluminum oxide alloy target prepared above as a rotary target, the Ar flow rate in the coating chamber is 220 sccm, the oxygen flow rate is 1.0 sccm, the vacuum degree of the coating chamber is between 3.8×10 -1 Pa, the total gas pressure is 0.30 Pa, the coating temperature is 350 °C, the thickness of the film obtained after coating is 1.1 nm, the resistance of the obtained coating product is 7×10 6 ohm, and the transmittance > 94.5%.

[0053] Example 3:

[0054] A preparation method of a zinc-aluminum oxide AZO alloy target:

[0055] S1. The capacity of the vacuum rolling mixer is 30.0 kg. Zinc oxide powder with a theoretical density of more than 98% and a Fisher average particle size of 7 μm and aluminum oxide powder with a theoretical density of more than 99.9% and a Fisher average particle size of 1 to 7 μm are selected respectively. The mass ratio of zinc oxide to aluminum oxide is 9:1. 27.00 kg of zinc oxide and 3.00 kg of aluminum oxide are weighed and put into a vacuum rolling mixer with a pressure of 2×10°Pa according to the mass ratio, and fully mixed at a speed of 80 r / min.

[0056] S2. Randomly select five points in the material mixed in step S1 to test the zinc oxide content and the aluminum oxide content, until the error of the zinc oxide content and the aluminum oxide content ratio at each test point is between 0.03%, and the mixing is completed;

[0057] S3, filling the mixed material treated in step S2 into a rubber sleeve equipped with a tubular flexible mold, and applying indium disulfide powder on the contact surface between the mold and the mixed material, then sealing the rubber sleeve and evacuating the vacuum, placing the evacuated rubber sleeve on a cold isostatic press, performing a primary pre-pressing at a pressure of 40 MPa to form a rough blank, performing a secondary pressing on the obtained rough blank at a pressure of 100 MPa until the density of the green blank reaches 62% of the theoretical density, and then releasing the pressure to normal pressure;

[0058] S4, placing the zinc-aluminum alloy target material green body pressed in step S3 in a vacuum hot pressing sintering furnace, hot pressing and sintering under the conditions of argon protection atmosphere, pressure of 30MPa and temperature of 1900°C, demolding at 600°C by a high temperature demolding process after keeping the temperature and pressure for 3 hours, cooling to room temperature, and obtaining a zinc oxide aluminum alloy target material crude product; machining the obtained zinc oxide aluminum alloy target material crude product to the required size, and then placing it in a vacuum annealing furnace, heating it to 1800°C and annealing it for 3 hours; performing chemical and physical tests, and then ultrasonically cleaning the target material to achieve a qualified roughness, and then processing and cleaning to obtain a zinc oxide aluminum alloy flat target material finished product;

[0059] S5, preparation of rotating target material: taking the mixed material after the treatment in step S2, and putting the mixed material into a ball mill for 3 hours, and passing through a 1000 mesh sieve to obtain zinc oxide aluminum spray powder;

[0060] In an inert gas protection atmosphere, a plasma spraying method is used to spray the outer surface of the S4 zinc oxide aluminum alloy flat target product with the obtained zinc oxide aluminum spray powder to obtain a target cavity;

[0061] The obtained target chamber is evacuated, and then an inert gas is introduced into it with a gas flow rate of 1200 sccm. Under the atmosphere of the inert gas, the aluminum zinc oxide spray powder is cold-sprayed into the inner cylindrical tube of the target chamber. The spraying thickness each time is 0.1 mm, and the total thickness reaches 11 mm. After that, a primary product of the (9:1) AZO alloy cylindrical target is obtained, and then the finished product of the aluminum zinc oxide alloy cylindrical target is obtained through processing and cleaning.

[0062] The aluminum zinc oxide alloy target prepared above is used as a rotating target. The Ar flow rate in the coating chamber is 220 sccm, the oxygen flow rate is 1.0 sccm, the vacuum degree in the coating chamber is between 4.0×10-1 Pa, the total gas pressure is 0.5 Pa, the coating temperature is 400 °C. After coating, the thickness of the obtained film is 1.4 nm, and the resistance of the obtained coating product is 8.9×10 6 ohms, and the transmittance > 94%.

[0063] In the above embodiments, the descriptions of each embodiment have their own focuses. For the parts not detailed or recorded in a certain embodiment, reference can be made to the relevant descriptions of other embodiments.

[0064] The above embodiments are only used to illustrate the technical solutions of the present application, rather than to limit it; although the present application has been described in detail with reference to the foregoing embodiments, those of ordinary skill in the art should understand that: they can still modify the technical solutions recorded in the foregoing embodiments, or perform equivalent replacements on some of the technical features; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of each embodiment of the present application, and should all be included in the protection scope of the present application.

Claims

1. A method for preparing a zinc oxide aluminum AZO alloy target, characterized in that: The following steps are involved: S1, mixing zinc oxide and aluminum oxide in a vacuum rolling mixer to obtain a mixture; S2, randomly selecting several locations in the mixed material to detect the contents of zinc oxide and aluminum oxide, until the mean error of the zinc oxide content and the aluminum oxide content at each detection point is lower than the error setting value; S3, filling the mixed material tested in S2 into a mold for pre-pressing to obtain a rough blank, and then performing secondary pressing on the rough blank to obtain a zinc oxide aluminum AZO alloy target green blank; S4, plane target material preparation: vacuum hot pressing and sintering the zinc oxide aluminum AZO alloy target green body, demolding, cooling to obtain a zinc oxide aluminum AZO alloy target rough product; machining the zinc oxide aluminum AZO alloy target rough product to a desired size, annealing, and cleaning to obtain a zinc oxide aluminum AZO alloy plane target; S5. Preparation of rotating target material: ball-mill and sieve the mixed material tested in S2 to obtain zinc oxide aluminum spraying powder, take the zinc oxide aluminum AZO alloy target green cylinder obtained in step S3, cold spray it onto the cylindrical target material, the spraying thickness is 0.1 mm each time, and spray multiple times to obtain an excellent rotating target material, and after processing, the zinc oxide aluminum AZO alloy rotating target material is obtained.

2. The preparation method according to claim 1, characterized in that: The mass ratio of zinc oxide to aluminum oxide in S1 is (5-9):(1-5), the Fisher average particle size of zinc oxide is 1-7 μm, and the Fisher average particle size of aluminum oxide is 1-7 μm.

3. The preparation method according to claim 1, characterized in that: As described in S1, the mixing is carried out in a vacuum tumbling mixer at a pressure of 2 Pa and a rotation speed of 50 to 80 r / min.

4. The preparation method according to claim 1, characterized in that: The error setting value in S2 is less than 0.03%.

5. The preparation method according to claim 1, characterized in that: The pre-pressing pressure in S3 is 10-60 MPa, the secondary pressing pressure is 50-200 MPa, and the density of the alloy target green body is 60-62% of the theoretical density.

6. The preparation method according to claim 1, characterized in that: The vacuum hot pressing sintering in S4 is carried out under an argon protective atmosphere, with a pressure of 20-30 MPa and a temperature of 1800-2000° C., and the temperature and pressure are kept constant for 3-4 hours; the demolding is carried out at 500-600° C.

7. The preparation method according to claim 1, characterized in that: The annealing conditions in S4 are: heating to 1800-1980° C. in a vacuum annealing furnace and annealing for 3-4 hours.

8. The preparation method according to claim 1, characterized in that: The ball milling was performed for 3-5 hours as described in S5, and the powder was passed through a 1000 mesh sieve to obtain AZO spray powder.