CoFeV alloy target material and preparation method thereof

Abstract

The invention belongs to the technical field of soft magnetic materials, and discloses a CoFeV alloy target material and a preparation method thereof. The preparation method comprises the following steps: carrying out vacuum induction melting and refining on a Co sheet, a Fe sheet and a V sheet, and then carrying out casting molding to obtain a CoFeV alloy ingot; the CoFeV alloy cast ingot is subjected to hot rolling treatment; a rough blank is obtained; performing water cutting on the rough blank to obtain a target blank; and the obtained target blank is machined through a grinding machine, the target blank with the flat and bright surface is obtained, finally, the target blank is welded to a copper back plate, and the CoFeV alloy target material is obtained. According to the preparation method, the CoFeV alloy target material is prepared through vacuum melting, and the preparation process conditions are further optimized, so that the quality of the CoFeV alloy target material can be remarkably improved, and the bonding rate of welding with a copper back plate is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of soft magnetic materials, and in particular relates to a CoFeV alloy target material and a preparation method thereof. Background Art

[0002] CoFeV soft magnetic alloy is a kind of excellent deformable permanent magnetic material. This kind of material can be made into thin cross-section or complex shape parts with different magnetic properties and high mechanical properties, so it occupies a unique position in the field of permanent magnetic materials. Deformable permanent magnetic materials are mainly used in magnetic compasses, aviation and automation instruments, hysteresis motor rotors, magnetic flip display systems, etc. Due to its excellent magnetic permeability, low coercive force and high saturation magnetic induction intensity, this kind of soft magnetic alloy plays a vital role in transformers, motors, relays and other equipment.

[0003] At present, the preparation method of CoFeV alloy target is mainly to prepare the target by pre-alloying some elements and then pulverizing them and hot pressing and sintering them with other elements. However, the obtained alloy target has problems such as low density, large porosity, high oxygen content, and low bonding rate with copper back plate.

[0004] Patent CN 102485948 A discloses a method for preparing a FeCoTaZr alloy sputtering target, which is obtained by vacuum induction melting (VIM) of four single elements Fe, Co, Ta, and Zr according to a ratio, and then the fully alloyed alloy melt is directly cast. It mainly uses a casting mold to control the cooling rate of the FeCoTaZr alloy solidification, ensures that the large-sized ingot will not break due to thermal stress during the solidification process, and forms a dispersed microstructure composed of an alloy phase rich in Ta and Zr elements and an FeCo alloy phase. However, the prior art does not disclose the preparation process conditions of the CoFeV soft magnetic alloy target, and how to improve the welding bonding rate with the copper backplane. Summary of the invention

[0005] In view of the shortcomings and deficiencies of the above prior art, the primary purpose of the present invention is to provide a method for preparing a CoFeV alloy target.

[0006] Another object of the present invention is to provide a CoFeV alloy target prepared by the above method.

[0007] The purpose of the present invention is achieved through the following technical solutions:

[0008] A method for preparing a CoFeV alloy target comprises the following preparation steps:

[0009] (1) Alloy smelting and refining: Co sheets, Fe sheets and V sheets are mixed and placed in a vacuum induction melting furnace for smelting and refining to obtain an alloy melt;

[0010] (2) Casting and cooling: casting the obtained alloy melt to obtain an alloy ingot;

[0011] (3) Thermal processing: hot rolling the CoFeV alloy ingot to obtain a rough billet;

[0012] (4) Water cutting: The rough blank is water cut to obtain the target blank;

[0013] (5) machining: subjecting the target blank obtained in step (4) to grinding to obtain a target blank with a smooth and bright surface;

[0014] (6) Welding: welding the target blank treated in step (5) to the copper backing plate to obtain a CoFeV alloy target.

[0015] Furthermore, the mass ratio (wt%) of the raw materials mixed in step (1) is 40-51% for Co sheets, 47-58% for Fe sheets, and 2% for V sheets.

[0016] Furthermore, the smelting and refining process in step (1) is first vacuumized to a pressure of 0.6 to 2.0×10 -2 Pa, and then filled with inert gas at a pressure of 0.04±0.02MPa.

[0017] Further preferably, the inert gas is argon, helium or nitrogen. More preferably, the inert gas is argon with a purity of ≥99.999%.

[0018] Furthermore, the smelting temperature in step (1) is 1600-1700° C., and the smelting time is 8-10 min.

[0019] Furthermore, the refining temperature in step (2) is 1500-1600° C., and the refining time is 5-6 min.

[0020] Furthermore, the hot rolling treatment in step (3) refers to multiple hot rolling treatments at 1000-1050°C.

[0021] Furthermore, in step (4), the feed rate of the water jet cutting is 15-25%, and the sand valve is adjusted to 95-100%.

[0022] Furthermore, the feed rate used in the grinding process in step (6) is ≤5 μm; the grinding wheel speed is ≤1800 r / min; under these parameters, it can be ensured that the oxidation of the target surface is minimized while the surface of the CoFeV target is effectively ground.

[0023] Furthermore, the bonding rate of the welding in step (7) is above 98%.

[0024] A CoFeV alloy target is prepared by the above preparation method.

[0025] Compared with the prior art, the present invention has the following beneficial effects:

[0026] (1) The method for preparing the CoFeV alloy target material of the present invention prepares the CoFeV alloy target material by vacuum melting, which can solve the technical problems of the CoFeV alloy target material prepared by the prior art, such as high oxygen content, uneven composition and unqualified appearance.

[0027] (2) The present invention can significantly improve the quality of the CoFeV alloy target and the bonding rate of the target with the copper back plate by further optimizing the preparation process conditions. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 This is a grain size distribution diagram of the CoFeV target material obtained in Example 1 of the present invention;

[0029] Figure 2 This is a graph showing the binding rate detection results of the CoFeV target material obtained in Example 1 of the present invention. DETAILED DESCRIPTION

[0030] The present invention is further described in detail below in conjunction with embodiments and drawings, but the embodiments of the present invention are not limited thereto.

[0031] Example 1

[0032] (1) Ingredients: According to the element composition by mass percentage: cobalt 49±0.2%, iron 49±0.2%, vanadium 2±0.2%, Co sheets and Fe sheets are mixed and placed alternately with V sheets into a small-sized water-cooled copper crucible with high magnetic induction strength in a vacuum induction melting furnace.

[0033] (2) Melting alloy: First, evacuate the vacuum induction melting furnace to 2×10 -2 Pa, fill the argon gas pressure to 0.04Mpa for protection to carry out CoFeV alloy smelting, add power to 300kw at 200kw / min, heat to 1600℃, wait for the material to be completely melted, smelt for 8min, cool with the furnace, and obtain CoFeV alloy ingot 01. Smelt in the same way to obtain CoFeV alloy ingot 02; then return CoFeV alloy ingot 01 and CoFeV alloy ingot 02 to the furnace, add power to 300kw at 200kw / min, heat to 1600℃, wait for the material to be completely melted, and refine for 8min, cool with the furnace, and obtain CoFeV alloy ingot 01 and CoFeV alloy ingot 02.

[0034] (3) Refining alloy: Place the smelted CoFeV alloy ingot 01 horizontally into a large-sized water-cooled copper crucible, and place the CoFeV alloy ingot 02 upside down into the water-cooled copper crucible, and evacuate to 2×10 -2 Pa, fill with argon protection, increase the power to 450kw at 200kw / min, raise the temperature to 1500℃, wait for the material to be completely melted, and then refine for 5min to obtain the alloy melt.

[0035] (4) Casting and cooling: After refining, the alloy melt is cast into a mold to form an alloy ingot. The mold size is the target blank size + 10 mm, and the height is 4 times the target blank thickness + 10 mm to obtain an alloy ingot.

[0036] (5) Hot rolling and hot isostatic pressing treatment: The target blank is hot rolled. After the furnace temperature rises to 1000°C, the target blank is placed in the furnace and heated for 1 hour. Each pass is 0.2 mm. After rolling 4 passes, it is kept at 1000°C for 10 minutes to eliminate shrinkage cavities and shrinkage inside the target blank and improve the density of the target material.

[0037] (6) Waterjet cutting: Cutting parameters: feed rate: 20% ± 5; sand valve adjustment: 90% -100%.

[0038] (7) Machining: The CoFeV alloy target blank is obtained by grinding. The feed amount of the grinding machine is ≤5 μm and the grinding wheel speed is 1800 r / min.

[0039] (8) Welding: The machined target blank is welded to the copper backing plate at a welding temperature of 180±5°C to obtain a CoFeV alloy target.

[0040] (9) Welding bonding rate inspection: Perform ultrasonic testing on the target material obtained after welding to confirm the welding bonding rate.

[0041] The size of the CoFeV alloy target prepared by this method reaches 300mm, the target is dense, the relative density is 99.9%, the target oxygen content is tested to be 27ppm, the carbon content is tested to be 8ppm, and the target composition is tested by sampling (as shown in Table 1), the component deviation is less than or equal to 0.05wt%, and the grain size is uniform (as shown in Table 1). Figure 1 As shown); the target binding rate is 99.2192% (as shown Figure 2 As shown), single point defect rate: 0.302%.

[0042] Table 1

[0043] project Co(wt%) Fe(wt%) V(wt%) Standard value 49±0.2％ 49±0.2％ 2±0.2％ Detection value 48.94％ 49.08％ 1.98％

[0044] Example 2

[0045] (1) Ingredients: Co sheets, Fe sheets and V sheets are placed alternately into a water-cooled copper crucible in a smelting furnace according to the element composition in percentage by mass: cobalt 45±0.2%, iron 53±0.2%, and vanadium 2±0.2%.

[0046] (2) Melting and refining alloy: First, evacuate the melting furnace to a vacuum of 1.8×10 -2 Pa, argon protection was used to melt the CoFeV alloy, the power was increased from 200kw / min to 300kw, the temperature was raised to 1600℃, and the material was refining for 10min after being completely melted.

[0047] (3) Casting and cooling: After refining, the alloy melt is cast into a mold to obtain an alloy target blank.

[0048] (4) Hot isostatic pressing treatment: The target blank is hot rolled, and after the furnace temperature is raised to 1000°C, the target blank is placed in the furnace and heated for 1 hour. This is a direct treatment to eliminate shrinkage cavities and shrinkage inside the target blank and improve the density of the target material.

[0049] (5) Waterjet cutting: Cutting parameters: feed rate: 15%; sand valve adjustment: 95%.

[0050] (6) Machining: The CoFeV alloy target blank is obtained by grinding. The feed amount of the grinding machine is ≤5 μm and the grinding wheel speed is 1800 r / min.

[0051] (7) Welding: Weld the machined target blank to the copper backing plate at a welding temperature of 175±5°C to obtain a CoFeV alloy target.

[0052] The target material components of this embodiment are shown in Table 2 through sampling and testing.

[0053] Table 2

[0054] project Co(wt%) Fe(wt%) V(wt%) Standard value 45±0.2％ 53±0.2％ 2±0.2％ Detection value 44.90％ 53.13％ 1.97％

[0055] Example 3

[0056] (1) Ingredients: According to the element composition by mass percentage: cobalt 40±0.2%, iron 58±0.2%, vanadium 2±0.2%, Co sheets and Fe sheets are mixed and placed in a water-cooled copper crucible in a smelting furnace in an alternating manner with V sheets.

[0057] (2) Melting alloy: First, evacuate the melting furnace to a vacuum of 2×10 -2 Pa, fill the argon gas pressure to 0.04Mpa for protection to carry out CoFeV alloy smelting, increase the power from 200kw / min to 300kw, raise the temperature to 1600℃, wait for the material to be completely melted, and then smelt for 8min, cool with the furnace to obtain CoFeV alloy ingot 01. Use the same method to smelt to obtain CoFeV alloy ingot 02;

[0058] (3) Refining alloy: Place the smelted CoFeV alloy ingot 01 horizontally into a water-cooled copper crucible, and place the CoFeV alloy ingot 02 upside down into a water-cooled copper crucible, and evacuate to 2×10 -2 Pa, fill with argon protection, increase the power to 450kw at 200kw / min, raise the temperature to 1500℃, wait for the material to be completely melted, and then refine for 5min to obtain the alloy melt.

[0059] (4) Casting and cooling: After refining, the alloy melt is cast into a mold to form a target blank. The mold size is the target blank size + 10 mm, and the height is 4 times the target blank thickness + 10 mm to obtain an alloy target blank.

[0060] (5) Hot isostatic pressing treatment: The target blank is hot rolled, and the furnace temperature is raised to 1000℃, and then the target blank is placed in the furnace and heated for 1 hour. Each pass is 0.2mm. After rolling 4 times, it is kept at 1000℃ for 10 minutes to eliminate shrinkage cavities and shrinkage inside the target blank and improve the density of the target material.

[0061] (6) Wire cutting: Cutting parameters: feed rate: 20%; sand valve adjustment: 100%.

[0062] (7) Machining: The CoFeV alloy target blank is obtained by grinding. The feed amount of the grinding machine is ≤5 μm and the grinding wheel speed is 1800 r / min.

[0063] (8) Welding: Welding the machined target blank to the copper backing plate at a welding temperature of 170±5°C to obtain a CoFeV alloy target.

[0064] The target material components of this embodiment are shown in Table 3 through sampling and testing.

[0065] Table 3

[0066] project Co(wt%) Fe(wt%) V(wt%) Standard value 40±0.2％ 58±0.2％ 2±0.2％ Detection value 40.12％ 57.90％ 1.98％

[0067] Example 4

[0068] (1) Ingredients: Co and V sheets are placed alternately in a water-cooled copper crucible in a smelting furnace according to the element composition by mass percentage: cobalt 51±0.2%, iron 47±0.2%, and vanadium 2±0.2%. Fe sheets are added through an external feeder.

[0069] (2) Melting alloy: First, evacuate the melting furnace to a vacuum of 2×10 -2 Pa, fill with argon pressure to 0.04Mpa for protection to carry out CoFeV alloy smelting, increase the power to 300kw at 200kw / min, raise the temperature to 1600℃, wait for the material to be completely melted, and then refine for 8min, cool with the furnace to obtain CoFeV alloy ingot.

[0070] (3) Refining the alloy: The smelted CoFeV alloy ingot was placed upside down in a water-cooled copper crucible and vacuumed to 2×10 -2 Pa, fill with argon protection, increase the power to 450kw at 200kw / min, raise the temperature to 1500℃, wait for the material to be completely melted, and then refine for 5min to obtain the alloy melt.

[0071] (4) Casting and cooling: After refining, the alloy melt is cast into a mold to obtain an alloy target blank.

[0072] (5) Hot rolling treatment: The target blank is hot rolled. After the furnace temperature rises to 1000°C, the target blank is placed in the furnace and heated for 1 hour. Each pass is 0.2 mm. After rolling 4 passes, the target blank is kept at 1000°C for 10 minutes.

[0073] (6) Waterjet cutting: Cutting parameters: feed rate: 25%; sand valve adjustment: 100%.

[0074] (7) Machining: The CoFeV alloy target blank is obtained by grinding. The feed amount of the grinding machine is ≤5 μm and the grinding wheel speed is 1800 r / min.

[0075] (8) Welding: Welding the machined target blank to the copper backing plate at a welding temperature of 170±5°C to obtain a CoFeV alloy target.

[0076] The target material components of this embodiment are shown in Table 4 through sampling and testing.

[0077] Table 4

[0078] project Co(wt%) Fe(wt%) V(wt%) Standard value 51±0.2％ 47±0.2％ 2±0.2％ Detection value 51.02％ 46.98％ 2.00％

[0079] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A method for preparing a CoFeV alloy target, characterized in that: The method comprises the following preparation steps: (1) Alloy smelting and refining: Co sheets, Fe sheets and V sheets are mixed and placed in a vacuum induction melting furnace for smelting and refining to obtain an alloy melt; (2) Casting and cooling: casting the obtained alloy melt to obtain an alloy ingot; (3) Thermal processing: hot rolling the CoFeV alloy ingot to obtain a rough billet; (4) Water cutting: The rough blank is water cut to obtain the target blank; (5) machining: subjecting the target blank obtained in step (4) to grinding to obtain a target blank with a smooth and bright surface; (6) Welding: welding the target blank treated in step (5) to the copper backing plate to obtain a CoFeV alloy target.

2. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The mass ratio of the raw materials mixed in step (1) is 40-51% of Co sheets, 47-58% of Fe sheets, and 2% of V sheets.

3. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: In the smelting and refining process of step (1), the evacuation is first performed to a pressure of 0.6 to 2.0×10 -2 Pa, and then filled with inert gas at a pressure of 0.04±0.02MPa.

4. The method for preparing a CoFeV alloy target according to claim 3, characterized in that: The inert gas is argon, helium or nitrogen.

5. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The smelting temperature in step (1) is 1600-1700° C., and the smelting time is 8-10 min.

6. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The refining temperature in step (2) is 1500-1600° C., and the refining time is 5-6 minutes.

7. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The hot rolling treatment in step (3) refers to multiple hot rolling treatments at 1000-1050°C.

8. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The feed rate of the water jet cutting in step (4) is 15-25%, and the sand valve is adjusted to 95-100%.

9. The method for preparing a CoFeV alloy target according to claim 1, characterized in that: The feed rate used in the grinding machine processing in step (5) is ≤5μm; the grinding wheel speed is ≤1800r / min.

10. A CoFeV alloy target, characterized in that: It is prepared by the preparation method according to any one of claims 1 to 9.

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