Europium barium copper oxide superconducting sputtering target material and preparation method thereof

Through the integrated molding-cold isostatic pressure and degreasing sintering treatment, the problem of density and microstructure uniformity control of the europium barium copper oxide superconducting sputtering target in the prior art is solved, and high density and low resistivity are achieved Eurobarium copper oxide superconducting sputtering target.

CN119285331APending Publication Date: 2025-01-10SUZHOU ZHICAI TECHNOLOGY CO LTD

Patent Information

Application Number
CN202411409009.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-10
Publication Date
2025-01-10

AI Technical Summary

Technical Problem

In the prior art, when preparing the europium barium copper oxide superconducting sputtering target, the pressure grouting molding operation is difficult to master, the drying and degreasing parameters are highly accurate and the period is long, resulting in difficult control of material density and microstructure uniformity.

Method used

The europium barium copper oxide target material blank was prepared by molding-cold isostatic pressing method, and the material density and microstructure uniformity were controlled by adjusting the molding and cold isostatic pressing pressure, combined with integrated degreasing and sintering, forming the main phase EuBa2Cu3O7 and the secondary phase CuO is uniformly dispersed.

Benefits of technology

The high relative density (97.98%) and low volume resistivity (1.98mΩ·cm) of the europium barium copper oxide superconducting sputtering target were achieved, which improved the densification degree and resistivity performance of the material.

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Abstract

The embodiment of the invention discloses a preparation method of a europium-barium-copper oxide superconducting sputtering target material, which comprises the following steps: mixing europium oxide powder, barium carbonate powder and barium oxide powder according to a set proportion, and then mixing with a dispersing agent and water to obtain first europium-barium-copper oxide slurry; carrying out spray granulation on the first europium-barium-copper oxide slurry to obtain first mixed powder; calcining the first mixed powder, and mixing the calcined first mixed powder with a dispersant, a binder and water to obtain second europium barium copper oxide slurry; performing spray granulation on the second europium-barium-copper oxide slurry to obtain second mixed powder; carrying out compression molding-cold isostatic pressing on the second mixed powder to obtain a europium-barium-copper oxide target material biscuit; wherein the mold pressing pressure ranges from 3 MPa to 6 MPa, and the cold isostatic pressing pressure ranges from 100 MPa to 250 MPa; the europium-barium-copper oxide target material biscuit is subjected to degreasing and sintering integrated treatment, and the europium-barium-copper oxide superconducting sputtering target material is obtained; the relative density of the europium barium copper oxide superconducting sputtering target material is as high as 97.98%, and the bulk resistivity is as low as 1.98 m omega.cm.
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Description

Technical Field

[0001] The invention belongs to the technical field of sputtering target materials, and in particular relates to a europium barium copper oxide superconducting sputtering target material and a preparation method thereof. Background Art

[0002] High-temperature superconducting materials have important potential applications in many fields such as microelectronics, transmission, superconducting devices, and magnetic energy storage due to their zero-resistance current transport characteristics at low temperatures. Among them, EBCO (rare earth barium copper oxide) high-temperature oxide superconducting materials have become one of the key research and development targets due to their relatively high critical transition temperature Tc, critical current density Jc, and rich physical properties.

[0003] There are three main forms of EBCO materials used in practical applications: strips, blocks and films. EBCO superconducting sputtering target itself is a ceramic material, which is brittle and easy to break, and difficult to process. Sputtering it into a film can solve this problem. EBCO strips and films are widely used. In order to prepare a superconducting film layer with high density, uniform structure and excellent superconducting performance, the superconducting sputtering target itself is required to have a high density and uniform microstructure. Therefore, the preparation of the superconducting sputtering target determines the performance of the superconducting film.

[0004] Patent document CN116606131A discloses a method for preparing a europium barium copper oxide target material, which mainly comprises mixing europium oxide powder, barium carbonate powder and copper oxide powder in a molar ratio of 1:4:6 and calcining them to make europium barium copper oxide slurry, and then subjecting them to pressure injection molding to obtain a europium barium copper oxide target material blank, and then subjecting them to drying treatment and degreasing and sintering treatment to obtain a uniform europium barium copper oxide superconducting sputtering target material. However, this method uses pressure injection molding to prepare the target material blank, and the injection operation is difficult to master, and the drying and degreasing parameters require high accuracy and a long cycle. Summary of the invention

[0005] In view of this, some embodiments disclose a method for preparing a europium barium copper oxide superconducting sputtering target, comprising:

[0006] Europium oxide powder, barium carbonate powder, and barium oxide powder are mixed in a set ratio, and then mixed with a dispersant and water to obtain a first europium barium copper oxide slurry; wherein the solid content of the first europium barium copper oxide slurry is 50-60%;

[0007] Spraying and granulating a first europium barium copper oxide slurry to obtain a first mixed powder;

[0008] The first mixed powder is calcined and then mixed with a dispersant, a binder and water to obtain a second europium barium copper oxide slurry; wherein the solid content of the second europium barium copper oxide slurry is 55%;

[0009] The second europium barium copper oxide slurry is sprayed and granulated to obtain a second mixed powder;

[0010] The second mixed powder is molded by molding and cold isostatic pressing to obtain a europium barium copper oxide target blank; wherein the molding pressure is 3-6 MPa, and the cold isostatic pressing pressure is 100-250 MPa; and the relative density of the europium barium copper oxide target blank is greater than 60%;

[0011] The europium barium copper oxide target blank is subjected to degreasing and sintering integration treatment to obtain a europium barium copper oxide superconducting sputtering target; the europium barium copper oxide superconducting sputtering target has a relative density of up to 97.98% and a volume resistivity as low as 1.98 mΩ·cm.

[0012] Furthermore, in some embodiments of the method for preparing a europium barium copper oxide superconducting sputtering target, the molar ratio of europium oxide powder, barium carbonate powder, and barium oxide powder is 1:4:6.

[0013] In some embodiments of the invention, the preparation method of europium barium copper oxide superconducting sputtering target is disclosed, wherein the europium oxide powder, barium carbonate powder and barium oxide powder are nano powders with a particle size distribution between 100 and 300 nm.

[0014] In some embodiments of the invention, the preparation method of europium barium copper oxide superconducting sputtering target is disclosed, wherein the europium oxide powder, the barium carbonate powder and the barium oxide powder are nano powders with a particle size distribution between 100 and 200 nm.

[0015] Some embodiments disclose a method for preparing a europium barium copper oxide superconducting sputtering target, in which the mass ratio of the dispersant, water and the first mixed powder in the first europium barium copper oxide slurry is 1.2-1.8:100-165:100; the rotation speed of the first europium barium copper oxide slurry spray granulation is 35-50 Hz, the air inlet temperature is 200-250°C, the air outlet temperature is 80-100°C, and the feed amount is 20-30%.

[0016] Some embodiments disclose a method for preparing a europium barium copper oxide superconducting sputtering target, in which the mass ratio of the dispersant, the binder, the water and the second mixed powder in the second europium barium copper oxide slurry is 1.2-1.8:0.5-1.0:100-165:100; the rotation speed of the second europium barium copper oxide slurry spray granulation is 35-50 Hz, the air inlet temperature is 200-250°C, the air outlet temperature is 80-100°C, and the feed amount is 20-30%.

[0017] In some embodiments of the method for preparing europium barium copper oxide superconducting sputtering target, the calcination treatment of the first mixed powder is carried out in an air atmosphere, the calcination temperature is 900-1000°C, the heating rate is 1-5°C / min, and the calcination time is 12-30h.

[0018] In some embodiments of the method for preparing a europium barium copper oxide superconducting sputtering target, the dispersant is polyacrylic acid or polycarboxylic acid dispersant, and the binder is polyvinyl alcohol, acrylic resin or gum arabic.

[0019] Some embodiments disclose a method for preparing a europium barium copper oxide superconducting sputtering target, wherein the degreasing and sintering integrated treatment of the europium barium copper oxide target blank comprises:

[0020] The degreasing temperature is 500-800°C, the degreasing heating rate is 0.5-1.5°C / min, and the degreasing holding time is 5-24h;

[0021] The sintering process is carried out according to the following step-by-step temperature sintering procedure:

[0022] The temperature was raised from room temperature to the first step temperature of 300°C at a heating rate of 0.5°C / min, and kept at the first step temperature for 10 h;

[0023] Continue to heat up to the second step temperature of 650°C at a heating rate of 0.5°C / min, and keep at the second step temperature for 20 hours;

[0024] Continue heating at a rate of 1°C / min to a third step temperature of 850-950°C, and keep at the third step temperature for 20 hours;

[0025] The temperature was lowered to the fourth step temperature of 500°C at a cooling rate of 1°C / min and kept at the fourth step temperature for 2h.

[0026] On the other hand, some embodiments disclose europium barium copper oxide superconducting sputtering targets, which are obtained by the preparation method of europium barium copper oxide superconducting sputtering targets disclosed in the embodiments of the present application. The relative density of the europium barium copper oxide superconducting sputtering targets is as high as 97.98%, and the bulk resistivity is as low as 1.98 mΩ·cm.

[0027] The method for preparing a europium barium copper oxide superconducting sputtering target disclosed in an embodiment of the present invention obtains a europium barium copper oxide superconducting sputtering target; a europium barium copper oxide target blank is prepared by a molding-cold isostatic pressing method, and the density and microstructure uniformity of the target blank are effectively controlled by adjusting the molding pressure and the cold isostatic pressing pressure. The pressure applied during the molding process directly affects the initial density and morphology of the material, and the cold isostatic pressing process further regulates the uniformity and density of the internal microstructure of the material; a main phase EuBa is formed in the europium barium copper oxide superconducting sputtering target obtained after degreasing and sintering integration treatment. 2 Cu 3 O 7The secondary phase CuO is evenly dispersed between the main phases, the europium barium copper oxide superconducting sputtering target has a uniform structure and a high degree of densification. The relative density of the europium barium copper oxide superconducting sputtering target is as high as 97.98%, and the volume resistivity is as low as 1.98mΩ·cm. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is the XRD diffraction pattern of the europium barium copper oxide superconducting sputtering target material of Example 1;

[0029] Figure 2 This is a SEM image of the europium barium copper oxide superconducting sputtering target of Example 1;

[0030] Figure 3 This is a grain structure distribution diagram of the europium barium copper oxide superconducting sputtering target material of Example 1;

[0031] Figure 3 In the figure, 1 represents the main phase grains of europium barium copper oxide, and 2 represents the copper oxide grains. DETAILED DESCRIPTION

[0032] The word "embodiment" used herein as an "exemplary" does not necessarily mean that any embodiment described is superior or better than other embodiments. Performance index tests in the embodiments of the present invention are performed using conventional test methods in the art unless otherwise specified. It should be understood that the terms described in the embodiments of the present invention are only used to describe specific implementation methods and are not intended to limit the contents disclosed in the embodiments of the present invention.

[0033] Unless otherwise specified, the technical and scientific terms used herein have the same meanings as commonly understood by ordinary technicians in the technical field to which the embodiments of the present invention belong; other experimental methods and technical means not specifically specified in the embodiments of the present invention refer to experimental methods and technical means commonly used by ordinary technicians in the field.

[0034] The terms "substantially" and "approximately" used herein are used to describe small fluctuations. For example, they can refer to less than or equal to ±5%, such as less than or equal to ±2%, such as less than or equal to ±1%, such as less than or equal to ±0.5%, such as less than or equal to ±0.2%, such as less than or equal to ±0.1%, such as less than or equal to ±0.05%. The numerical data represented or presented in the range format herein are used only for convenience and brevity, and should therefore be flexibly interpreted as including not only the values ​​clearly listed as the limits of the range, but also all independent values ​​or sub-ranges contained in the range. For example, the numerical range of "1-5%" should be interpreted as including not only the clearly listed values ​​of 1% to 5%, but also the independent values ​​and sub-ranges within the range shown. Therefore, independent values ​​such as 2%, 3.5% and 4% and sub-ranges such as 1%-3%, 2%-4% and 3%-5% are included in this numerical range. This principle also applies to the range of only one numerical value. In addition, such an interpretation applies regardless of the width of the range or the characteristics described.

[0035] In this document, including in the claims, transitional words such as "comprises," "includes," "with," "having," "containing," "involving," "accommodating," etc. are understood to be open-ended, i.e., meaning "including but not limited to." Only the transitional words "consisting of" and "composed of" are closed transitional words.

[0036] In order to better illustrate the present invention, numerous specific details are provided in the specific examples below. It should be understood by those skilled in the art that the present invention can be implemented without certain specific details. In the embodiments, some methods, means, instruments, equipment, etc. well known to those skilled in the art are not described in detail in order to highlight the gist of the present invention.

[0037] Under the premise of no conflict, the technical features disclosed in the embodiments of the present invention may be arbitrarily combined, and the resulting technical solutions belong to the contents disclosed in the embodiments of the present invention.

[0038] In some embodiments, a method for preparing a europium barium copper oxide superconducting sputtering target comprises:

[0039] Europium oxide powder, barium carbonate powder, and barium oxide powder are mixed in a set ratio, and then mixed with a dispersant and water to obtain a first europium barium copper oxide slurry; wherein the solid content in the first europium barium copper oxide slurry is 50-60%; usually, the dispersant is a polyacrylic acid or a polycarboxylic acid dispersant; wherein the solid content refers to the mass content of the oxide powder in the first europium barium copper oxide slurry;

[0040] Spraying and granulating a first europium barium copper oxide slurry to obtain a first mixed powder;

[0041] The first mixed powder is calcined and then mixed with a dispersant, a binder and water to obtain a second europium barium copper oxide slurry; wherein the solid content of the second europium barium copper oxide slurry is 55%; generally, the dispersant is polyacrylic acid or polycarboxylic acid dispersant, and the binder is polyvinyl alcohol, acrylic resin or gum arabic; the solid content refers to the mass content of the oxide powder in the second europium barium copper oxide slurry;

[0042] The second europium barium copper oxide slurry is sprayed and granulated to obtain a second mixed powder;

[0043] The second mixed powder is molded by molding-cold isostatic pressing to obtain a europium barium copper oxide target blank, and the relative density of the europium barium copper oxide target blank is greater than 60%; generally, molding-cold isostatic pressing is an effective method for preparing superconducting sputtering targets. By adjusting the molding pressure and the cold isostatic pressing pressure, the density and microstructure uniformity of the target blank can be significantly affected; the pressure applied during the molding process directly affects the initial density and morphology of the material, and the cold isostatic pressing process further regulates the uniformity and density of the internal microstructure of the material; as an optional embodiment, the molding pressure is 3-6MPa, and the cold isostatic pressing pressure is 100-250MPa;

[0044] The europium barium copper oxide target blank is subjected to an integrated degreasing and sintering process to obtain a europium barium copper oxide superconducting sputtering target; the relative density of the europium barium copper oxide superconducting sputtering target is as high as 97.98%, and the volume resistivity is as low as 1.98mΩ·cm. Generally, the integrated degreasing and sintering process refers to the continuous degreasing and sintering processes. After the europium barium copper oxide target blank is degreasingly treated, the temperature is continuously raised to the sintering temperature at the degreasing temperature, and the sintering process is performed according to the set sintering process to obtain the europium barium copper oxide superconducting sputtering target;

[0045] In some embodiments, the molar ratio of europium oxide powder, barium carbonate powder, and barium oxide powder is 1:4:6.

[0046] In some embodiments, the europium oxide powder, the barium carbonate powder, and the barium oxide powder are nanopowders with a particle size distribution between 100 and 300 nm.

[0047] In some preferred embodiments, the europium oxide powder, the barium carbonate powder and the barium oxide powder are nanopowders with a particle size distribution between 100 and 200 nm.

[0048] In some embodiments, the mass ratio of the dispersant, water and the first mixed powder in the first europium barium copper oxide slurry is 1.2-1.8:100-165:100; the rotation speed of the first europium barium copper oxide slurry spray granulation is 35-50 Hz, the air inlet temperature is 200-250°C, the air outlet temperature is 80-100°C, and the feed amount is 20-30%.

[0049] In some embodiments, the mass ratio of the dispersant, binder, water and the second mixed powder in the second europium barium copper oxide slurry is 1.2-1.8:0.5-1.0:100-165:100; the rotation speed of the second europium barium copper oxide slurry spray granulation is 35-50 Hz, the air inlet temperature is 200-250°C, the air outlet temperature is 80-100°C, and the feed amount is 20-30%.

[0050] In some embodiments, the calcination of the first mixed powder is carried out in an air atmosphere, the calcination temperature is 900-1000° C., the heating rate is 1-5° C. / min, and the calcination time is 12-30 h.

[0051] Some embodiments disclose a method for preparing a europium barium copper oxide superconducting sputtering target, wherein the degreasing and sintering integrated treatment of the europium barium copper oxide target blank comprises:

[0052] The degreasing temperature is 500-800°C, the degreasing heating rate is 0.5-1.5°C / min, and the degreasing holding time is 5-24h;

[0053] The sintering process is carried out according to the following step-by-step temperature sintering procedure:

[0054] The temperature was raised from room temperature to the first step temperature of 300°C at a heating rate of 0.5°C / min, and kept at the first step temperature for 10 h;

[0055] The temperature was raised from the first step temperature to the second step temperature of 650°C at a heating rate of 0.5°C / min, and kept at the second step temperature for 20 hours;

[0056] The temperature was raised from the second step temperature to the third step temperature of 850-950°C at a heating rate of 1°C / min, and kept at the third step temperature for 20 hours;

[0057] The temperature was cooled from the third step temperature to the fourth step temperature of 500°C at a cooling rate of 1°C / min, and kept at the fourth step temperature for 2h.

[0058] The technical details are further illustrated below in conjunction with embodiments.

[0059] Example 1

[0060] In Example 1, the method for preparing the europium barium copper oxide superconducting sputtering target comprises:

[0061] Europium oxide powder, barium carbonate powder and barium oxide powder with a particle size distribution between 100 and 300 nm are mixed in a molar ratio of 1:4:6, with a total mass of 1300 g; then mixed with 10 g of dispersant polyacrylic acid and 300 g of deionized water to obtain a first europium barium copper oxide slurry; wherein the solid content in the first europium barium copper oxide slurry is 55%;

[0062] The first europium barium copper oxide slurry is spray granulated to obtain a first mixed powder; the spray granulation speed is 40HZ, the air inlet temperature is 230°C, the air outlet temperature is 90°C, the feed amount is 21.9%, and 1200g of the first mixed powder is obtained after spray granulation;

[0063] The first mixed powder is calcined at 900°C in an air atmosphere, with a heating rate of 2°C / min and a calcination time of 20h;

[0064] The calcined europium barium copper oxide powder is pulverized and classified by air flow mill, and then mixed with 12g of polyacrylic acid as a dispersant, 5g of polyvinyl alcohol as a binder and 300g of water to obtain a second europium barium copper oxide slurry; wherein the solid content of the second europium barium copper oxide slurry is 55%;

[0065] The second europium barium copper oxide slurry was dispersed by functional sand milling at a sand mill speed of 1800 rpm for 60 min, and then spray granulated to obtain 1000 g of the second mixed powder; the spray granulation speed was 40 Hz, the air inlet temperature was 230° C., the air outlet temperature was 90° C., and the feed amount was 22.5%;

[0066] The second mixed powder is molded by molding and cold isostatic pressing to obtain a europium barium copper oxide target blank; wherein the molding pressure is 4.5 MPa, the cold isostatic pressing pressure is 100 MPa; the relative density of the europium barium copper oxide target blank is 60%;

[0067] The europium barium copper oxide target blank is subjected to degreasing and sintering integrated treatment to obtain the europium barium copper oxide superconducting sputtering target; the integrated treatment process includes:

[0068] The temperature was raised to 600°C, a degreasing temperature, at a heating rate of 1.0°C / min and kept at this temperature for 12 hours;

[0069] The sintering process is carried out according to the following step-by-step temperature sintering procedure:

[0070] The temperature was raised from room temperature to the first step temperature of 300°C at a heating rate of 0.5°C / min, and kept at the first step temperature for 10 h;

[0071] The temperature was raised from 300°C to the second step temperature of 650°C at a heating rate of 0.5°C / min, and kept at the second step temperature for 20 hours;

[0072] The temperature was raised from 650°C to the third step temperature of 920°C at a heating rate of 1°C / min, and kept at the third step temperature for 20 hours;

[0073] Cool down from 920°C to the fourth step temperature of 500°C at a cooling rate of 1°C / min, and keep at the fourth step temperature for 2h;

[0074] Then, the temperature is naturally lowered and cooled to obtain a europium barium copper oxide superconducting sputtering target;

[0075] The relative density of the europium barium copper oxide superconducting sputtering target is as high as 97.24%, and the bulk resistivity is as low as 2.14 mΩ·cm.

[0076] The europium barium copper oxide superconducting sputtering target obtained in Example 1 was tested, wherein the XRD diffraction pattern of the europium barium copper oxide superconducting sputtering target is as follows: Figure 1 As shown, the scanning electron microscope image of the cross section of the europium barium copper oxide superconducting sputtering target is as follows Figure 2 As shown, the target material is fully densified; the grain structure distribution diagram of the superconducting sputtering target material of europium barium copper oxide is shown in Figure 3 As shown, the main phase grains 1 in the europium barium copper oxide superconducting sputtering target are europium barium copper oxide, and copper oxide grains 2 are discretely and evenly distributed between the europium barium copper oxide main phase grains 1; the grains 2 are completely filled between the main phase grains 1, and the target material has a high degree of densification.

[0077] It can be seen that the oxide powder in the europium barium copper oxide target blank forms the main phase EuBa after degreasing and sintering process. 2 Cu 3 O 7 The secondary phase CuO is evenly dispersed between the main phases to obtain a europium barium copper oxide superconducting sputtering target with uniform structure, high relative density and low resistivity.

[0078] Example 2

[0079] In Example 2, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the cold isostatic pressing pressure is 150 MPa.

[0080] The europium barium copper oxide superconducting sputtering target obtained in Example 2 was tested, and the results are listed in Table 1.

[0081] Example 3

[0082] In Example 3, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the cold isostatic pressing pressure is 250 MPa.

[0083] The europium barium copper oxide superconducting sputtering target obtained in Example 3 was tested, and the results are listed in Table 1.

[0084] Example 4

[0085] In Example 4, the preparation method of europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the particle size of europium oxide powder, barium carbonate powder and copper oxide powder is nanometer scale, the particle size distribution is between 100 and 200 nm, and the rotation speed of the high-energy sand mill is 2000 rpm.

[0086] The europium barium copper oxide superconducting sputtering target obtained in Example 4 was tested, and the results are listed in Table 1.

[0087] Comparative Example 1

[0088] In Comparative Example 1, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the cold isostatic pressing pressure is 50 MPa.

[0089] The europium barium copper oxide superconducting sputtering target obtained in this comparative example 1 was tested, and the results are listed in Table 1.

[0090] Comparative Example 2

[0091] In Comparative Example 2, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the molding pressure is 3 MPa and the cold isostatic pressing pressure is 50 MPa.

[0092] The europium barium copper oxide superconducting sputtering target obtained in this comparative example 2 was tested, and the results are listed in Table 1.

[0093] Comparative Example 3

[0094] In Comparative Example 3, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the molding pressure is 6 MPa and the cold isostatic pressing pressure is 50 MPa.

[0095] The europium barium copper oxide superconducting sputtering target obtained in this comparative example 3 was tested, and the results are listed in Table 1.

[0096] Comparative Example 4

[0097] In Comparative Example 4, the preparation method of the europium barium copper oxide superconducting sputtering target material refers to Example 1; wherein the molding pressure is 4.5 MPa and the cold isostatic pressing pressure is 0 MPa.

[0098] The europium barium copper oxide superconducting sputtering target obtained in Comparative Example 4 was tested, and the results are listed in Table 1.

[0099] Table 1 Properties of Europium Barium Copper Oxide Superconducting Sputtering Targets

[0100]

[0101] The method for preparing a europium barium copper oxide superconducting sputtering target disclosed in an embodiment of the present invention obtains a europium barium copper oxide superconducting sputtering target; a europium barium copper oxide target blank is prepared by a molding-cold isostatic pressing method, and the density and microstructure uniformity of the target blank are effectively controlled by adjusting the molding pressure and the cold isostatic pressing pressure. The pressure applied during the molding process directly affects the initial density and morphology of the material, and the cold isostatic pressing process further regulates the uniformity and density of the internal microstructure of the material; after degreasing and sintering integrated treatment, a europium barium copper oxide superconducting sputtering target is obtained, and a main phase EuBa is formed in the target. 2 Cu 3 O 7 The secondary phase CuO is evenly dispersed between the main phases, the internal structure of the europium barium copper oxide superconducting sputtering target is uniform and the degree of densification is high. The relative density of the europium barium copper oxide superconducting sputtering target is as high as 97.98%, and the volume resistivity is as low as 1.98mΩ·cm.

[0102] The technical solutions disclosed in the embodiments of the present invention and the technical details disclosed in the embodiments are merely illustrative of the inventive concept of the present invention and do not constitute a limitation on the technical solutions of the embodiments of the present invention. Any conventional changes, replacements or combinations of the technical details disclosed in the embodiments of the present invention have the same inventive concept as the present invention and are within the protection scope of the claims of the present invention.

Claims

1. A method for preparing a superconducting sputtering target of europium barium copper oxide, characterized in that: include: Europium oxide powder, barium carbonate powder, and barium oxide powder are mixed in a set ratio, and then mixed with a dispersant and water to obtain a first europium barium copper oxide slurry; wherein the solid content of the first europium barium copper oxide slurry is 50-60%; Spraying and granulating a first europium barium copper oxide slurry to obtain a first mixed powder; The first mixed powder is calcined and then mixed with a dispersant, a binder and water to obtain a second europium barium copper oxide slurry; wherein the solid content of the second europium barium copper oxide slurry is 55%; The second europium barium copper oxide slurry is sprayed and granulated to obtain a second mixed powder; The second mixed powder is molded by molding and cold isostatic pressing to obtain a europium barium copper oxide target blank; wherein the molding pressure is 3-6 MPa, and the cold isostatic pressing pressure is 100-250 MPa; and the relative density of the europium barium copper oxide target blank is greater than 60%; The europium barium copper oxide target blank is subjected to degreasing and sintering integration treatment to obtain a europium barium copper oxide superconducting sputtering target; the europium barium copper oxide superconducting sputtering target has a relative density of up to 97.98% and a volume resistivity as low as 1.98 mΩ·cm.

2. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The molar ratio of europium oxide powder, barium carbonate powder and barium oxide powder is 1:4:

6.

3. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The europium oxide powder, barium carbonate powder and barium oxide powder are nano powders with a particle size distribution between 100 and 300 nm.

4. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The europium oxide powder, barium carbonate powder and barium oxide powder are nano powders with a particle size distribution between 100 and 200 nm.

5. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: In the first europium barium copper oxide slurry, the mass ratio of dispersant, water and first mixed powder is 1.2-1.8:100-165:100; the rotation speed of the first europium barium copper oxide slurry spray granulation is 35-50Hz, the air inlet temperature is 200-250℃, the air outlet temperature is 80-100℃, and the feed amount is 20-30%.

6. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: In the second europium barium copper oxide slurry, the mass ratio of the dispersant, the binder, the water and the second mixed powder is 1.2-1.8:0.5-1.0:100-165:100; the rotation speed of the second europium barium copper oxide slurry spray granulation is 35-50Hz, the air inlet temperature is 200-250℃, the air outlet temperature is 80-100℃, and the feed amount is 20-30%.

7. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The calcination treatment of the first mixed powder is carried out in an air atmosphere, the calcination temperature is 900-1000° C., the heating rate is 1-5° C. / min, and the calcination time is 12-30 hours.

8. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The dispersant is polyacrylic acid or polycarboxylic acid dispersant, and the binder is polyvinyl alcohol, acrylic resin or gum arabic.

9. The method for preparing the europium barium copper oxide superconducting sputtering target according to claim 1, characterized in that: The integrated degreasing and sintering process of Europium Barium Copper Oxide target blank includes: The degreasing temperature is 500-800°C, the degreasing heating rate is 0.5-1.5°C / min, and the degreasing holding time is 5-24h; The sintering process is carried out according to the following step-by-step temperature sintering procedure: The temperature was raised from room temperature to the first step temperature of 300°C at a heating rate of 0.5°C / min, and kept at the first step temperature for 10 h; Continue heating at a rate of 0.5°C / min to the second step temperature of 650°C, and keep at the second step temperature for 20 hours; Continue heating at a rate of 1°C / min to the third step temperature of 850-950°C, and keep at the third step temperature for 20 hours; The temperature was lowered to the fourth step temperature of 500°C at a cooling rate of 1°C / min and kept at the fourth step temperature for 2h.

10. Europium barium copper oxide superconducting sputtering target, characterized in that: The preparation method according to any one of claims 1 to 9 obtains the europium barium copper oxide superconducting sputtering target material, the relative density of which is as high as 97.98%, and the volume resistivity of which is as low as 1.98 mΩ·cm.

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