CN113235058B - Preparation method of CoZrTa alloy target blank and target material - Google Patents
Preparation method of CoZrTa alloy target blank and target material Download PDFInfo
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- CN113235058B CN113235058B CN202110498032.9A CN202110498032A CN113235058B CN 113235058 B CN113235058 B CN 113235058B CN 202110498032 A CN202110498032 A CN 202110498032A CN 113235058 B CN113235058 B CN 113235058B
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- 239000013077 target material Substances 0.000 title claims abstract description 31
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 24
- 239000000956 alloy Substances 0.000 title claims abstract description 24
- 229910019586 CoZrTa Inorganic materials 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000000155 melt Substances 0.000 claims abstract description 25
- 238000005096 rolling process Methods 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 15
- 238000003723 Smelting Methods 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000005266 casting Methods 0.000 claims abstract description 9
- 238000012545 processing Methods 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052802 copper Inorganic materials 0.000 claims abstract description 5
- 239000010949 copper Substances 0.000 claims abstract description 5
- 238000004519 manufacturing process Methods 0.000 claims abstract description 5
- 238000000465 moulding Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 5
- 238000003754 machining Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000005098 hot rolling Methods 0.000 claims description 6
- 238000003303 reheating Methods 0.000 claims description 4
- 230000035699 permeability Effects 0.000 abstract description 14
- 230000008569 process Effects 0.000 abstract description 11
- 238000002844 melting Methods 0.000 description 20
- 230000008018 melting Effects 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 15
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 12
- 238000001816 cooling Methods 0.000 description 12
- 238000012360 testing method Methods 0.000 description 9
- ZGWQKLYPIPNASE-UHFFFAOYSA-N [Co].[Zr].[Ta] Chemical compound [Co].[Zr].[Ta] ZGWQKLYPIPNASE-UHFFFAOYSA-N 0.000 description 7
- 229910052786 argon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000010408 film Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- 238000009826 distribution Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000004544 sputter deposition Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
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- 239000000243 solution Substances 0.000 description 3
- 229910052715 tantalum Inorganic materials 0.000 description 3
- 229910020641 Co Zr Inorganic materials 0.000 description 2
- 229910020520 Co—Zr Inorganic materials 0.000 description 2
- 229910001093 Zr alloy Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010894 electron beam technology Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005242 forging Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
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- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- 229910001362 Ta alloys Inorganic materials 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000001513 hot isostatic pressing Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/04—Influencing the temperature of the metal, e.g. by heating or cooling the mould
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/11—Making amorphous alloys
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/07—Alloys based on nickel or cobalt based on cobalt
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C45/00—Amorphous alloys
- C22C45/04—Amorphous alloys with nickel or cobalt as the major constituent
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C2200/00—Crystalline structure
- C22C2200/02—Amorphous
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Abstract
The invention discloses a preparation method of a CoZrTa alloy target blank and a target, and relates to the field of target preparation. The invention provides a preparation method of a CoZrTa alloy target blank, which comprises the following steps: (1) weighing required raw materials according to a ratio, wherein the raw materials comprise Co sheets, Ta sheets and Zr particles, according to a layer-by-layer stacking mode, the bottom layer and the uppermost layer are Co sheets, and the middle Ta sheet layer and the Zr particle layer cannot be adjacent layers, and placing the raw materials in a water-cooled copper crucible; (2) vacuumizing the crucible, increasing power, keeping the power stable when no insoluble substances in the melt roll, carrying out magnetic suspension smelting, and then preserving heat to obtain the melt; (3) and (3) casting the melt obtained in the step (2) into a mold for molding, and obtaining the CoZrTa alloy after preliminary processing and rolling. Compared with the traditional process, the invention obviously improves the production efficiency, reduces the target material cost, and achieves the high magnetic permeability of 65 percent when the target material thickness is 4 mm.
Description
Technical Field
The invention relates to the field of target preparation, in particular to a CoZrTa alloy target blank and a preparation method of a target.
Background
As electronic systems have been developed to have high integration and high complexity, it is necessary to integrate more components on smaller substrates. Besides the development of high-density integration technology, the development of miniaturized and thin-film devices from the devices themselves to reduce the overall volume and weight of the system is undoubtedly a feasible approach. An Inductor (Inductor) is a component that can convert electrical energy into magnetic energy for storage. The film inductor is an inductor manufactured by adopting a vacuum film process, has high reliability, is easy to integrate and chip, is very suitable for an automatic Surface Mount Technology (SMT), and has become a hot spot of domestic and foreign research due to the advantages of small size, good high-frequency characteristic and the like. The thin film inductor can effectively improve inductance and reduce the size of a device due to the introduction of the magnetic thin film, effectively improves the high-frequency performance of the inductor, opens an effective way for the miniaturization and high-frequency of the inductor, and becomes the mainstream of the future inductor. Among the materials of choice for current thin film inductors, the Co-based series and Fe-based series are the most common. The Co-based series includes CoNbZr amorphous soft magnetic films, CoPdSiO granular films and CoTaZr amorphous films.
CN20191114936.X a preparation method and application of a cobalt-tantalum-zirconium alloy target, the patent controls the organization structure and target performance of the alloy by composition design, high vacuum vertical melting and high vacuum electron beam melting, three-dimensional isothermal hot forging cogging, variable angle control rolling process and the like, and the high-quality cobalt-tantalum-zirconium alloy target is prepared. It is also mentioned in this patent that the selection of a particular texture orientation can improve the magnetic properties of a high purity cobalt tantalum zirconium target. At present, the grain distribution and the phase structure distribution of the cobalt-tantalum-zirconium target material are still lack of effective control, and the use efficiency and the sputtering film-forming performance of the target material are not facilitated. The magnetic permeability is an important index for checking the sputtering performance of the target, and the magnetic target with high magnetic permeability can concentrate a magnetic field in the target as much as possible, so that the glow process is more stable, and therefore, the sputtering film-forming performance under vacuum can be improved by improving the magnetic permeability vertical to the target surface. The blank obtained by the conventional medium-frequency induction vacuum melting has coarse grains, is easy to generate a banded structure, and reduces the sputtering performance of the target.
The existing method for preparing the cobalt-zirconium-tantalum alloy target requires a hot isostatic pressing device or a method combining high-temperature refining and low-temperature refining or a high-vacuum vertical melting and high-vacuum electron beam melting, three-dimensional isothermal hot forging cogging and variable-angle control rolling process, is relatively complicated and is not beneficial to batch production. And when the target is round, the preparation process has the problems of raw material waste and the like.
Disclosure of Invention
Based on the above, the invention aims to overcome the defects of the prior art and provide a method for preparing a CoZrTa alloy target blank and a target material, which avoid a complicated smelting process, have higher magnetic permeability and lower cost.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: a preparation method of a CoZrTa alloy target blank comprises the following steps:
(1) weighing required raw materials according to a ratio, wherein the raw materials comprise Co sheets, Ta sheets and Zr particles, according to a layer-by-layer stacking mode, the bottom layer and the uppermost layer are Co sheets, and the middle Ta sheet layer and the Zr particle layer cannot be adjacent layers, and placing the raw materials in a water-cooled copper crucible;
(2) vacuumizing the crucible, increasing power, keeping the power stable when no insoluble substances in the melt roll, carrying out magnetic suspension smelting, and then preserving heat to obtain the melt;
(3) and (3) casting the melt obtained in the step (2) into a mold for molding, and obtaining the CoZrTa alloy target blank after preliminary processing and rolling.
The invention provides a preparation method of a CoZrTa alloy target blank, which can ensure that a uniform melt can be obtained by one-time smelting by adopting a specific feeding mode, and avoid a complicated smelting process. Compared with the traditional process, the preparation method provided by the application has the advantages that the production efficiency is remarkably improved, and the cost is reduced.
Preferably, in the step (1), the purity of the raw material is more than 4N; in the raw materials, the mass percentages of the Co sheet, the Ta sheet and the Zr particles are respectively as follows: 80-84wt% of Co sheet, 5-12wt% of Ta sheet and 4-15wt% of Zr particles. Further preferably, the thickness of the Co sheet is 3-8mm, and the length and the width of the Co sheet are both less than 4 cm; the thickness of the Ta sheet is 1-3mm, and the length and the width of the Ta sheet are both less than 3 cm; the grain diameter of the Zr particles is 3-10 mm.
The invention adopts a specific feeding mode to ensure that uniform melt can be obtained by one-time smelting, thereby avoiding a complicated smelting process. The alloy system smelted by the invention mainly comprises three elements of Co, Zr and Ta, wherein the melting point of Co is 1492 ℃, the melting point of Zr is 1852 ℃ and the melting point of Ta is 2996 ℃. The Co sheet accounts for about 82 wt%, Zr particles with a high melting point and Ta sheets are separated from each other up and down by using the Co sheet with a low melting point according to the feeding mode, in the induction heating process of the suspension smelting furnace, the Co sheet with the low melting point is firstly absorbed and melted by induced current and flows into the surfaces of Zr and Ta with high melting points in a molten liquid state mode, and Co melt slowly permeates the surface of a simple substance with the high melting point to form an intermetallic compound or solid solution of Co-Zr and Co-Ta; such as Co 7 Ta 2 (950 ℃), greatly reduces the melting temperature and shortens the melting time. Compared with the mixed feeding of three simple substances of Co, Zr and TaIn the material feeding mode, after the low-melting-point Co is completely melted, the high-melting-point simple substance is sunk into the melt to be slowly soaked and melted, the melting mode is long in time consumption, and due to the fact that the specific material feeding mode provided by the application does not have a high-melting-point simple substance gathering area, heating power consumption can be fully absorbed, the melting speed is high, and the melt is more uniform.
Preferably, in the step (2), the degree of vacuum in the crucible after evacuation is 2.0 × 10 -2 Pa; the rate of increasing power is 50-100Kw/min, and the final stable power is 350-450 Kw; the temperature for heat preservation is 1375 and 1420 ℃, and the time for heat preservation is 8-10 min. The vacuum degree in the crucible after vacuum pumping is 2.0 multiplied by 10 -2 And Pa, filling argon gas to wash the furnace, vacuumizing again, and then refilling argon gas to protect, wherein the furnace pressure is 0.06 MPa.
Preferably, in the step (3), the mold is a water-cooled mold, the water pressure of the water-cooled mold is 0.24-0.32MPa, the water temperature is 8-10 ℃, and the casting time is 5-8 s. Further preferably, in the step (3) described in the present application, the melt obtained in the step (2) needs to be rapidly cast into a mold, the melt is rapidly cooled by rapidly and forcibly cooling the high-temperature melt, the water-cooled mold is used as shown in fig. 1, amorphous and highly oriented grains can be effectively formed by cooling from bottom to top, and the magnetic permeability of the target after subsequent rolling processing is higher.
In addition, the present application provides a target blank prepared according to the above-described method for preparing a target blank.
Further, the present application provides a method for preparing a target material using the above target blank, the method comprising: machining the target blank to ensure the target blank to be flat up and down; carrying out hot rolling on the flattened target blank to obtain a plate blank; and (4) carrying out thermal leveling and machining on the plate blank to obtain the target material.
Preferably, the machining is to machine away the raised portion on the target blank and ensure that the target blank is flat on top of the other. Further preferably, the protruding part is machined by a lathe after being cut by a sawing machine, so that the target blank is ensured to be flat up and down.
Preferably, the target is a circular target; the hot rolling process comprises the following specific steps: and heating the target blank to 950-1150 ℃, preserving heat for 0.5-1h, reducing by 0.25-2mm according to each pass, and reheating for 10-15min after rolling for 4 passes in each cycle to obtain the plate blank. Further preferably, the rolling direction is arbitrary, the roundness of the target material is ensured, the roundness of the target material is measured in the rolling process, and the target material can be rolled along the direction until the target material is in a perfect circle when the size is smaller.
Compared with the prior art, the invention has the beneficial effects that: this application adopts special feeding mode, can ensure once to smelt and just can obtain even fuse-element, avoids loaded down with trivial details smelting process. The method has the advantages that the melt is rapidly cooled in a manner of rapidly and forcibly cooling the high-temperature melt, amorphous and highly oriented grains can be effectively formed by cooling from bottom to top, and the magnetic permeability of the target material after subsequent rolling processing is higher. Compared with the traditional process, the invention obviously improves the production efficiency, reduces the target material cost and achieves high magnetic permeability of 65 percent.
Drawings
FIG. 1 is a diagram of a water cooled mold; wherein, 1 is a water inlet, and 2 is a water outlet;
FIG. 2 is a pictorial representation of a target blank and target material prepared in example 1; wherein, figure (a) is a CoZrTa alloy target blank, and figure (b) is a target material;
FIG. 3 is a gold phase diagram of the target of example 1.
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to the accompanying drawings and specific embodiments.
Example 1
In an embodiment of the present application, the method for preparing a target according to the embodiment includes the following steps:
(1) weighing the required raw materials according to the proportion, calculating the required metal Co of 16.70Kg and Ta of 1.12Kg according to the theoretical proportion of the CoZrTa alloy, and Zr: 2.52Kg of a mass, the total weight amounting to 20.356Kg, wherein the Co sheet is divided into 10 parts, the Ta sheet is divided into 4 parts, and the Zr particles are divided into 4 parts, which are placed in a water-cooled copper crucible according to a specific feeding mode, the feeding mode is Co-Zr-Co-Ta-Co-Zr-Co-Ta-Co;
(2) the power is increased after the crucible is vacuumized,when no insoluble substances in the melt roll, keeping the power stable, and carrying out magnetic suspension smelting and then preserving the heat to obtain the melt; wherein the vacuum degree in the crucible after vacuum pumping is 2.0 multiplied by 10 -2 Pa, filling argon gas to wash the furnace, vacuumizing again, and then refilling argon gas to protect, wherein the furnace pressure is 0.06 MPa; the speed of increasing the power is 100Kw/min, the melt in the crucible starts to roll and melt, materials continuously start to melt, when no insoluble substances roll in the melt, the power is kept stable, and the final stable power is 350-450 Kw; the temperature for heat preservation is 1420 ℃, and the time for heat preservation is 8 min;
(3) quickly casting the melt obtained in the step (2) into a mold for molding, wherein the mold is a water-cooling mold, the water pressure of the water-cooling mold is 0.24MPa, the water temperature is 8 ℃, and the casting time is 8s, so as to obtain the target blank;
(4) machining the target blank to ensure the target blank to be flat up and down; carrying out hot rolling on the flattened target blank to obtain a plate blank; machining the plate blank to obtain the target material; during mechanical processing, the raised part on the target blank is completely demoulded by a sawing machine to obtain the target blank with the periphery processed completely to be smooth and free of defects; measuring the size of a target blank to be 167.18mm multiplied by 52.29mm, placing the target blank in a muffle furnace, heating to 1050 ℃, keeping the temperature for 1h, reducing the thickness by 0.25mm according to each pass, rolling for 4 passes, reheating for 10min, and obtaining a plate blank in any direction of rolling direction; and after the last rolling is finished, quickly flattening the plate blank under a hydraulic press, cooling, and machining to obtain the cobalt-zirconium-tantalum target material with the required size (the diameter is 450mm x 4 mm).
Example 2
In an embodiment of the present application, the method for preparing a target according to the embodiment includes the following steps:
(1) weighing the required raw materials according to the proportion, calculating the required metal Co of 16.70Kg and Ta of 1.12Kg according to the theoretical proportion of the CoZrTa alloy, and Zr: 2.52Kg of a mass, the total weight amounting to 20.356Kg, wherein 5 parts of Co sheet, 2 parts of Ta sheet and 2 parts of Zr particles are placed in a water-cooled copper crucible according to a specific feeding mode, and the feeding mode is Co-Ta-Co-Zr-Co;
(2) the power is increased after the crucible is vacuumized,when no insoluble substances in the melt roll, keeping the power stable, and carrying out magnetic suspension smelting and then preserving the heat to obtain the melt; wherein the vacuum degree in the crucible after vacuum pumping is 2.0 multiplied by 10 -2 Pa, filling argon gas to wash the furnace, vacuumizing again, and then refilling argon gas to protect, wherein the furnace pressure is 0.06 MPa; the speed of increasing the power is 50Kw/min, the melt in the crucible starts to roll and melt, materials continuously start to melt, when no insoluble substances roll in the melt, the power is kept stable, and the final stable power is 350-450 Kw; the heat preservation temperature is 1375 ℃, and the heat preservation time is 10 min;
(3) quickly casting the melt obtained in the step (2) into a mold for molding, wherein the mold is a water-cooled mold, the water pressure of the water-cooled mold is 32MPa, the water temperature is 10 ℃, and the casting time is 5s, so as to obtain the target blank;
(4) machining the target blank to ensure the target blank to be flat up and down; carrying out hot rolling on the flattened target blank to obtain a plate blank; machining the plate blank to obtain the target material; during mechanical processing, the raised part on the target blank is completely demoulded by a sawing machine to obtain the target blank with the periphery processed completely to be smooth and free of defects; measuring the size of a target blank to be 167.18mm multiplied by 52.29mm, placing the target blank in a muffle furnace, heating to 1050 ℃, keeping the temperature for 1h, reducing the thickness by 0.25mm according to each pass, rolling for 4 passes, reheating for 10min, and obtaining a plate blank in any direction of rolling direction; and after the last rolling is finished, quickly flattening the plate blank under a hydraulic press, cooling, and machining to obtain the cobalt-zirconium-tantalum target material with the required size (the diameter is 450mm multiplied by 4 mm).
Fig. 2 shows the actual diagrams of the target blank (left) and the target (right) prepared in example 1 of the present application, and fig. 3 shows the metallographic diagram of the target prepared in example 1. According to a metallographic phase, the crystal grains of the target material are in an amorphous ribbon structure, and the size distribution and the phase distribution of the crystal grains are uniform; the physical map and the golden picture in embodiment 2 are similar to those in embodiment 1, and are not repeated herein.
Meanwhile, the application is provided with comparative examples, and the specific comparative examples are as follows:
compared with the example 1, the comparative example 1 is different from the example 1 only in feeding mode, the comparative example 1 is a mixed feeding mode, and the selection, content and preparation method of the rest components are the same as those in the example 1;
compared with the example 1, the comparative example 2 is different only in feeding mode, the feeding mode of the comparative example 2 is layer-by-layer superposition, the feeding mode is Co-Ta-Zr-Co-Ta-Zr-Co, and the selection, content and preparation method of the rest components are the same as those of the example 1;
compared with the example 1, the comparative example 3 is different only in feeding mode, the feeding mode of the comparative example 3 is layer-by-layer superposition, the feeding mode is Ta-Co-Zr-Co-Ta-Co-Zr, and the selection, content and preparation method of the other components are the same as those of the example 1;
compared with the embodiment 1, the comparative example 4 has different cooling modes in the step (3), the melted melt is directly cast into a graphite mold, and the target blank is obtained by natural cooling without cooling by cooling water.
Test example target Density test
The testing process comprises the following steps: processing the target material to the size of a finished product, taking small blocks along different three positions of the edge to test the component content, impurity content and density of Co, Zr and Ta, and simultaneously placing the small blocks on a platform to test the magnetic permeability by adopting a gauss meter.
And (4) testing standard: the magnetic permeability is implemented by the regulation of industry standard YS/T1124, the relative density of the product is implemented according to national standard GB/T3850,
and (3) testing results: the test results are shown in table 1:
TABLE 1 target test results
| Purity of target material | Time of melting | Uniformity of composition | Magnetic permeability | Relative density | |
| Example 1 | 3.5N | Short length | Good taste | 65％ | 99％ |
| Example 2 | 3.5N | Short length | Good taste | 60％ | 99％ |
| Comparative example 1 | 3.5N | Long and long | Difference (D) | 30％ | 98％ |
| Comparative example 2 | 3.5N | Long and long | Difference (D) | 40％ | 99％ |
| Comparative example 3 | 3.5N | Long and long | Difference between | 32％ | 99％ |
| Comparative example 4 | 3.5N | Short length | Good taste | 25％ | 97％ |
As can be seen from Table 1, the comparative examples 1 to 3 differ from the present application only in the feeding manner, and the final result is that the melt composition is not uniform, and the uniform composition effect of our example 1 can be achieved by multiple melting or long-time melting without adopting the feeding manner specified in the present application. This is also a problem that is not overcome by the current target material preparation process. The cooling mode of the comparative example 4 is different from that of the present application, and the magnetic permeability is only 25%, which is greatly different from that of the present application; according to the embodiment of the application, the target material is cooled from bottom to top, amorphous and highly oriented grains can be effectively formed, and the magnetic permeability of the target material is higher after subsequent rolling processing. The target material prepared by the embodiment of the application avoids a fussy smelting process, and when the thickness of the target material is 4mm, the magnetic permeability is as high as more than 60%, and the cost is low.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. The preparation method of the CoZrTa alloy target blank is characterized by comprising the following steps:
(1) weighing required raw materials according to a ratio, wherein the raw materials comprise Co sheets, Ta sheets and Zr particles, according to a layer-by-layer stacking mode, the bottom layer and the uppermost layer are Co sheets, and the middle Ta sheet layer and the Zr particle layer cannot be adjacent layers, and placing the raw materials in a water-cooled copper crucible;
(2) vacuumizing the crucible, increasing power, keeping the power stable when no insoluble substances in the melt roll, carrying out magnetic suspension smelting, and then preserving heat to obtain the melt;
(3) casting the melt obtained in the step (2) into a mold for molding, and obtaining the CoZrTa alloy target blank after preliminary processing and rolling; the mold is a water-cooled mold, and is cooled from bottom to top, the water pressure of the water-cooled mold is 0.24-0.32MPa, the water temperature is 8-10 ℃, and the casting time is 5-8 s.
2. The method of making a target blank of a CoZrTa alloy according to claim 1, wherein in step (1), the raw material purity is greater than 4N; the mass percentages of the Co sheet, the Ta sheet and the Zr particles in the raw materials are respectively as follows: 80-84wt% of Co sheet, 5-12wt% of Ta sheet and 4-15wt% of Zr particles.
3. The method of making a target blank of a CoZrTa alloy according to claim 2, wherein the thickness of the Co sheet is 3-8mm, and the length and width are less than 4 cm; the thickness of the Ta sheet is 1-3mm, and the length and the width of the Ta sheet are both less than 3 cm; the grain diameter of the Zr particles is 3-10 mm.
4. The method of producing a target blank of a CoZrTa alloy as claimed in claim 1, wherein in the step (2), the degree of vacuum in the crucible after evacuation is 2.0X 10 -2 Pa; the rate of increasing power is 50-100kW/min, and the final stable power is 350-450 kW; the temperature for heat preservation is 1375 and 1420 ℃, and the time for heat preservation is 8-10 min.
5. A CoZrTa alloy target blank produced by the method of producing a CoZrTa alloy target blank according to any one of claims 1 to 4.
6. A method for preparing a target material by using the CoZrTa alloy target blank according to claim 5, wherein the method comprises the following steps: machining the CoZrTa alloy target blank to ensure that the target blank is flat up and down; carrying out hot rolling on the flattened target blank to obtain a plate blank; and (4) carrying out thermal leveling and machining on the plate blank to obtain the target material.
7. The method of claim 6, wherein the machining is performed by machining a raised portion of the target blank to ensure that the target blank is flat on top of the target blank.
8. The method for preparing a target according to claim 6, wherein the target is a circular target; the hot rolling process comprises the following specific steps: and heating the target blank to 950-1150 ℃, preserving heat for 0.5-1h, reducing by 0.25-2mm according to each pass, and reheating for 10-15min after rolling for 4 passes in each cycle to obtain the plate blank.
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| WO2004043631A1 (en) * | 2002-11-07 | 2004-05-27 | Honeywell International Inc. | Die cast sputter targets |
| JP2017119904A (en) * | 2015-12-28 | 2017-07-06 | Ｊｘ金属株式会社 | Sputtering target made of cobalt or cobalt base alloy, and production method thereof |
| CN110735068A (en) * | 2019-11-21 | 2020-01-31 | 中南大学 | A kind of preparation method of cobalt tantalum zirconium alloy target and application thereof |
| CN111424245A (en) * | 2020-04-24 | 2020-07-17 | 先导薄膜材料（广东）有限公司 | Preparation method of cobalt-tantalum-zirconium target material |
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| WO2004043631A1 (en) * | 2002-11-07 | 2004-05-27 | Honeywell International Inc. | Die cast sputter targets |
| JP2017119904A (en) * | 2015-12-28 | 2017-07-06 | Ｊｘ金属株式会社 | Sputtering target made of cobalt or cobalt base alloy, and production method thereof |
| CN110735068A (en) * | 2019-11-21 | 2020-01-31 | 中南大学 | A kind of preparation method of cobalt tantalum zirconium alloy target and application thereof |
| CN111424245A (en) * | 2020-04-24 | 2020-07-17 | 先导薄膜材料（广东）有限公司 | Preparation method of cobalt-tantalum-zirconium target material |
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