Copper-iron-chromium-nickel quaternary alloy planar sputtering target and preparation method thereof

The copper-iron-chromium-nickel quadrimer alloy plane sputtering target was prepared through vacuum induction smelting and hot rolling molding, which solved the problem of insufficient corrosion resistance and mechanical properties of the alloy sputtering target, and achieved high purity and high performance alloy targets.

CN116607026BActive Publication Date: 2025-08-19PILOT FILM MATERIAL TECHNOLOGY SINGAPORE CO LTD
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Patent Information

Application Number
CN202310592526.2
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-05-24
Publication Date
2025-08-19
Estimated Expiration
2043-05-24

AI Technical Summary

Technical Problem

The corrosion resistance and mechanical properties of existing alloy sputtering targets are poor.

Method used

The copper, iron, chromium and nickel quadrimer alloy planar sputtering target is prepared by vacuum induction smelting method. By smelting copper, iron, chromium and nickel raw materials in a vacuum induction smelting furnace, a high-density molded target is formed, and the conductivity, thermal conductivity and mechanical strength of the alloy are improved through hot rolling molding and machining.

Benefits of technology

The corrosion resistance and mechanical properties of the alloy sputtering target are significantly improved, ensuring that the purity of the molded target reaches more than 99.99%.

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Abstract

The present invention discloses a copper-iron-chromium-nickel quaternary alloy planar sputtering target and a preparation method thereof. The preparation method comprises at least a vacuum induction melting and casting step: copper, iron, chromium, and nickel raw materials are placed in a vacuum induction melting furnace according to a preset mass ratio to form a shaped target material, wherein the shaped target material has a relative density of not less than 99%. Since the shaped target material is melted in the vacuum induction melting furnace, the copper, iron, chromium, and nickel raw materials disclosed in the present invention can be fully fused in the vacuum induction melting furnace. Moreover, since the copper-iron alloy has good electrical and thermal conductivity, high mechanical strength, and wear resistance, the addition of chromium can further improve the corrosion resistance and mechanical properties of the alloy. The addition of nickel can fully cooperate with chromium to transform the metallographic structure from a single-phase ferrite to a two-phase structure of austenite and ferrite, thereby effectively improving the corrosion resistance and mechanical properties of the alloy target material.
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Description

Technical Field

[0001] The present invention relates to the technical field of powder metallurgy, and in particular to a copper-iron-chromium-nickel quaternary alloy sputtering target and a preparation method thereof. Background Art

[0002] There are many alloy planar sputtering targets on the market, such as copper-manganese-aluminum alloy sputtering targets, nickel-platinum alloy targets, and cobalt-chromium-platinum-boron-rhenium sputtering targets. However, due to problems such as processing methods and the alloy itself, the above alloy targets have poor corrosion resistance and mechanical properties.

[0003] Therefore, how to effectively improve the corrosion resistance and mechanical properties of alloy sputtering targets is a technical problem that needs to be urgently solved by those skilled in the art. Summary of the Invention

[0004] In view of this, the object of the present invention is to provide a method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target, which can effectively improve the corrosion resistance and mechanical properties of the alloy sputtering target.

[0005] Another object of the present invention is to provide a copper-iron-chromium-nickel quaternary alloy planar sputtering target.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] A method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target material comprises at least a vacuum induction melting and casting step:

[0008] Copper, iron, chromium and nickel raw materials are placed in a vacuum induction melting furnace according to a preset mass ratio to be processed into a shaped target material, and the relative density of the shaped target material is not less than 99%.

[0009] Preferably, the vacuum induction melting casting step comprises:

[0010] Raw material melting: placing the copper, iron, chromium and nickel raw materials into a preparation device and heating them to a first preset temperature, so that the copper, iron, chromium and nickel raw materials are melted into a copper-iron-chromium-nickel molten material;

[0011] Material pouring: pouring the copper, iron, chromium and nickel molten material into a mold, and vacuuming the mold to make the vacuum value of the mold reach a preset vacuum value;

[0012] Cooling and demolding: cooling the copper, iron, chromium and nickel molten material to room temperature in the mold and then demolding to obtain the formed target material.

[0013] Preferably, the preset mass ratio of the copper, iron, chromium and nickel raw materials is (80-100%): (0-20%): (0-5%): (0-5%).

[0014] Preferably, the first preset temperature is 1000°C-2000°C; and / or

[0015] The preset vacuum value is less than 10 -4 Pa.

[0016] Preferably, the method further comprises the steps of:

[0017] Hot rolling forming: After preheating the forming target material to a second preset temperature, the forming target material is rolled into a preset finished target material.

[0018] Preferably, in the hot rolling forming step, the second preset temperature is 600°C-900°C.

[0019] Preferably, in the hot rolling forming step, the forming target material is unidirectionally rolled along the length direction.

[0020] Preferably, the vacuum induction melting casting step further includes a raw material preparation step:

[0021] Copper bars, iron bars, chromium powder and nickel powder are selected as the copper, iron, chromium and nickel raw materials, and the purity of the copper bars, iron bars, chromium powder and nickel powder is greater than 99.99%.

[0022] Preferably, the method further comprises the steps of:

[0023] Machining to remove defects, warped parts and machining allowances of the formed target material; and / or,

[0024] Quality inspection, testing and analyzing the molding target material to obtain the grain size, phase distribution and impurity element content of the molding target material; and / or,

[0025] Polishing treatment to remove mechanical scratches and fingerprints on the molding target material so that the smoothness of the molding target material is within a preset smoothness range; and / or,

[0026] Packaging treatment: Packaging treatment is performed on the molding target material.

[0027] A copper-iron-chromium-nickel quaternary alloy planar sputtering target is prepared by any of the above methods for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target, wherein the purity of the copper-iron-chromium-nickel quaternary alloy planar sputtering target is greater than or equal to 99.99%.

[0028] It can be seen from the above technical solution that since the formed target material is melted in a vacuum induction melting furnace, the copper, iron, chromium and nickel raw materials disclosed in the embodiment of the present invention can be fully fused in the vacuum induction melting furnace. Moreover, since the copper-iron alloy has good electrical conductivity, thermal conductivity, high mechanical strength, hardness and wear resistance, the addition of chromium can further improve the corrosion resistance and mechanical properties of the alloy. The addition of nickel can fully cooperate with the chromium element to change the metallographic structure from a single-phase ferrite to a two-phase structure of austenite and ferrite, thereby effectively improving the corrosion resistance and mechanical properties of the alloy target. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the following briefly introduces the drawings required for use in the embodiments or the description of the prior art. Obviously, the drawings described below are merely embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on the provided drawings without paying any creative work.

[0030] Figure 1 A schematic flow chart of a method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the first embodiment of the present invention;

[0031] Figure 2 Schematic diagram of the process of preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the second embodiment of the present invention;

[0032] Figure 3 A schematic flow chart of a method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in a third embodiment of the present invention;

[0033] Figure 4 Schematic diagram of the process of preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the fourth embodiment of the present invention;

[0034] Figure 5 This is a schematic cross-sectional SEM diagram of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention;

[0035] Figure 6 This is a schematic diagram of the main structure of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention;

[0036] Figure 7 This is a schematic side view of the structure of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention.

[0037] The names of the components are as follows:

[0038] 100 is the forming target. DETAILED DESCRIPTION

[0039] In view of this, the core of the present invention is to provide a method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target, which can effectively improve the corrosion resistance and mechanical properties of the alloy sputtering target.

[0040] Another core of the present invention is to provide a copper-iron-chromium-nickel quaternary alloy planar sputtering target.

[0041] In order to make those skilled in the art better understand the present invention, the present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. Figures 1 to 7 .

[0042] Example 1:

[0043] Please refer to Figure 1 The preparation method of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention includes at least a vacuum induction melting and casting step, wherein the vacuum induction melting and casting step is to place copper, iron, chromium and nickel raw materials according to a preset mass ratio into a vacuum induction melting furnace to process them into a shaped target material 100, and the relative density of the shaped target material 100 is not less than 99%.

[0044] Since the formed target material 100 is melted in a vacuum induction melting furnace, the copper, iron, chromium and nickel raw materials disclosed in the embodiment of the present invention can be fully fused in the vacuum induction melting furnace. Moreover, since the copper-iron alloy has good electrical conductivity, thermal conductivity, high mechanical strength, hardness and wear resistance, the addition of chromium can further improve the corrosion resistance and mechanical properties of the alloy. The addition of nickel can fully cooperate with the chromium element to change the metallographic structure from a single-phase ferrite to a two-phase structure of austenite and ferrite, thereby effectively improving the corrosion resistance and mechanical properties of the alloy target.

[0045] The embodiments of the present invention do not limit the specific steps of vacuum induction melting casting. As long as the structure meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0046] As a preferred embodiment, the vacuum induction melting casting steps disclosed in the embodiment of the present invention include raw material melting, material pouring and cooling and demolding steps, wherein the raw material melting step is to place the copper, iron, chromium and nickel raw materials into a preparation device and heat them to a first preset temperature, so that the copper, iron, chromium and nickel raw materials are melted into copper-iron-chromium-nickel molten materials, the material pouring step is to pour the copper-iron-chromium-nickel molten materials into the mold, and vacuum the mold so that the vacuum value of the mold is a preset vacuum value, and the cooling and demolding step is to cool the copper-iron-chromium-nickel molten materials in the mold to room temperature and then demold to obtain a formed target material 100.

[0047] When preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target, first, the copper, iron, chromium and nickel raw materials need to be placed in a preparation device and heated to a first preset temperature, so that the copper, iron, chromium and nickel raw materials are melted into a copper-iron-chromium-nickel molten material, and then the copper-iron-chromium-nickel molten material is poured into a mold, and the mold is vacuumed so that the vacuum value of the mold is a preset vacuum value. Finally, the copper-iron-chromium-nickel molten material is cooled to room temperature in the mold and demolded to obtain a formed target 100.

[0048] The embodiments of the present invention do not specifically limit the preparation device. As long as the structure meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0049] As a preferred embodiment, the preparation device disclosed in the embodiment of the present invention preferably uses a zirconia crucible.

[0050] The embodiment of the present invention does not limit the preset mass ratio of copper, iron, chromium and nickel raw materials. As long as the mass ratio meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0051] As a preferred embodiment, the preset mass ratio of the copper, iron, chromium and nickel raw materials disclosed in the embodiment of the present invention is (80-100%): (0-20%): (0-5%): (0-5%).

[0052] Experiments have shown that the corrosion resistance and mechanical properties of the formed target material 100 formed by melting the copper, iron, chromium and nickel raw materials formed under the above mass ratio in a vacuum induction melting furnace can be further improved.

[0053] The embodiment of the present invention does not limit the specific value of the first preset temperature. As long as the value meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0054] As a preferred embodiment, the first preset temperature disclosed in the embodiment of the present invention is 1000°C-2000°C.

[0055] The embodiment of the present invention does not limit the specific numerical value of the preset vacuum value. As long as the numerical value meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0056] As a preferred embodiment, the preset vacuum value disclosed in the embodiment of the present invention is preferably less than 10 -4 Pa.

[0057] Example 2:

[0058] Please refer to Figure 2As a further preferred embodiment, the method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the embodiment of the present invention further includes a hot rolling forming step, wherein the hot rolling forming step is to preheat the formed target 100 to a second preset temperature and then roll the formed target 100 into a preset finished target.

[0059] After the preparation of the formed target material 100 is completed, the formed target material 100 needs to be preheated to a second preset temperature, and then rolled into a preset finished target material according to actual needs.

[0060] The embodiment of the present invention does not limit the specific value of the second preset temperature. As long as the value meets the use requirements of the present invention, it is within the protection scope of the present invention.

[0061] As a preferred embodiment, the second preset temperature disclosed in the embodiment of the present invention is 600°C-900°C.

[0062] It should be noted that, in the hot rolling forming step disclosed in the embodiment of the present invention, the formed target material 100 needs to be unidirectionally rolled along the length direction to obtain the preset finished target material.

[0063] Example 3:

[0064] Please refer to Figure 3 As a further preferred embodiment, the method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention further includes a raw material preparation step before the vacuum induction melting casting step, wherein the raw material preparation step is to select copper bars, iron bars, chromium powder and nickel powder as copper, iron, chromium and nickel raw materials, and the purity of the copper bars, iron bars, chromium powder and nickel powder is greater than 99.99%.

[0065] Example 4:

[0066] Please refer to Figure 4 As a further preferred embodiment, the method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention further includes a machining step, wherein the machining step is to remove defects, warped parts and processing allowances of the formed target 100.

[0067] The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention also includes a quality inspection step, wherein the quality inspection step is to inspect and analyze the formed target 100 to obtain the grain size, phase distribution and impurity element content of the formed target 100.

[0068] The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention further comprises: polishing deal withSteps, wherein the polishing step is to remove mechanical scratches and fingerprints on the molding target 100, so that the smoothness of the molding target 100 is within a preset smoothness range.

[0069] The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention further includes a packaging process step, wherein the packaging process is to perform packaging process on the formed target 100 .

[0070] As a more specific embodiment, the method for preparing the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the embodiment of the present invention specifically includes:

[0071] Raw material preparation: Copper bars, iron bars, chromium and nickel powders are selected as raw materials, and the purity of copper bars, iron bars, chromium powder and nickel powder should all be greater than 99.99%. Samples are sent to the laboratory for incoming material testing. Copper bars and stainless steel bars are cut into small pieces and chromium and nickel powders are weighed. The raw materials are mixed according to the mass ratio of copper: iron: chromium: nickel = 79:16:3:2;

[0072] Vacuum induction melting treatment: After copper, iron, chromium and nickel raw materials are filled into a zirconia crucible, the whole is placed in a vacuum induction melting furnace at a temperature of 1500°C to melt the copper, iron, chromium and nickel raw materials into a copper-iron-chromium-nickel molten material. The copper-iron-chromium-nickel molten material is then poured into a mold, and the mold is evacuated to a vacuum value of less than 10-4Pa. Finally, the copper-iron-chromium-nickel molten material is cooled to room temperature in the mold and demolded to obtain a formed target material;

[0073] Hot rolling treatment: After the shaped target material 100 is prepared, it is necessary to preheat the shaped target material 100 to 600°C-900°C, and then roll the shaped target material 100 into a preset finished target material according to actual needs;

[0074] Machining: remove defects, warping and machining allowances of the preset finished target material;

[0075] Quality inspection step: Detect and analyze the preset finished target material to obtain the grain size, phase distribution and impurity element content of the preset finished target material;

[0076] Polishing: to remove mechanical scratches and fingerprints on the preset finished target material so that the finish of the preset finished target material is within the preset finish range;

[0077] Packaging: Packaging the preset finished target materials.

[0078] The present invention also discloses a copper-iron-chromium-nickel quaternary alloy planar sputtering target, please refer to Figure 5-Figure 7 ,in Figure 5 This is a cross-sectional SEM diagram of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention (magnified 500 times). Figure 6This is a schematic diagram of the main structure of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention. Figure 7 This is a side structural schematic diagram of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in an embodiment of the present invention. The above-mentioned copper-iron-chromium-nickel quaternary alloy planar sputtering target is prepared using the preparation method of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in any of the above-mentioned embodiments.

[0079] Since the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the above embodiment is prepared using the preparation method of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the above embodiment, the above copper-iron-chromium-nickel quaternary alloy planar sputtering target has the technical advantages of the preparation method of the copper-iron-chromium-nickel quaternary alloy planar sputtering target disclosed in the above embodiment.

[0080] The purity of the copper-iron-chromium-nickel quaternary alloy planar sputtering target prepared by the above preparation method is greater than or equal to 99.99%.

[0081] In the description of this application, it should be noted that the terms "first" and "second" are used for descriptive purposes only and should not be understood as indicating or implying relative importance.

[0082] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target, characterized in that: At least includes vacuum induction melting and casting steps: The copper, iron, chromium and nickel raw materials are placed in a vacuum induction melting furnace according to a preset mass ratio to form a shaped target material, wherein the relative density of the shaped target material is not less than 99%; The vacuum induction melting casting step comprises: Raw material melting: placing the copper, iron, chromium and nickel raw materials into a preparation device and heating them to a first preset temperature, so that the copper, iron, chromium and nickel raw materials are melted into a copper-iron-chromium-nickel molten material; Material pouring: pouring the copper, iron, chromium and nickel molten material into a mold, and vacuuming the mold to make the vacuum value of the mold reach a preset vacuum value; Cooling and demolding: cooling the copper, iron, chromium and nickel molten material to room temperature in the mold and then demolding to obtain the formed target material; The preset mass ratio of the copper, iron, chromium and nickel raw materials is 79:16:3:

2.

2. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 1, characterized in that: The first preset temperature is 1000° C.-2000° C.; and / or The preset vacuum value is less than 10 -4 Pa.

3. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 1, characterized in that: Also includes the steps: Hot rolling forming: After preheating the forming target material to a second preset temperature, the forming target material is rolled into a preset finished target material.

4. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 3, characterized in that: In the hot rolling forming step, the second preset temperature is 600°C-900°C.

5. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 3, characterized in that: In the hot rolling forming step, the forming target material is unidirectionally rolled along the length direction.

6. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 1, characterized in that: The vacuum induction melting casting step also includes a raw material preparation step: Copper bars, iron bars, chromium powder and nickel powder are selected as the copper, iron, chromium and nickel raw materials, and the purity of the copper bars, iron bars, chromium powder and nickel powder is greater than 99.

99.

7. The method for preparing a copper-iron-chromium-nickel quaternary alloy planar sputtering target according to claim 6, characterized in that: Also includes the steps: Machining to remove defects, warped parts and machining allowances of the formed target material; and / or, Quality inspection, testing and analyzing the molding target material to obtain the grain size, phase distribution and impurity element content of the molding target material; and / or, Polishing treatment to remove mechanical scratches and fingerprints on the molding target material so that the smoothness of the molding target material is within a preset smoothness range; and / or, Packaging treatment: Packaging treatment is performed on the molding target material.

8. A copper-iron-chromium-nickel quaternary alloy planar sputtering target, characterized in that: The copper-iron-chromium-nickel quaternary alloy planar sputtering target is prepared by the preparation method of the copper-iron-chromium-nickel quaternary alloy planar sputtering target according to any one of claims 1 to 7, and the purity of the copper-iron-chromium-nickel quaternary alloy planar sputtering target is greater than or equal to 99.9%.

Citation Information

Patent Citations

  • Method for producing copper sputtering target material

    CN101509125A