Preparation method of high-purity low-oxygen AlTi alloy target material

Abstract

The invention discloses a preparation method of a high-purity and low-oxygen AlTi alloy target material, relates to the field of sputter coating, and aims to solve the problem of how to prepare the high-purity and low-oxygen AlTi alloy target material. The preparation method is characterized by comprising the following steps that S1, an Al wire and a Ti wire are adopted as raw materials, and the diameter ratio of the Al wire to the Ti wire is 3: 1; s2, the Al wire and the Ti wire are subjected to acid pickling treatment through a cleaning agent, ultrasonic cleaning is conducted for 30-60 min through clear water after acid pickling, drying is conducted after cleaning, and the wires are installed on a vacuum arc equipment mechanical arm wire feeding disc after drying; s3, the back pipe is subjected to surface sand blasting roughening treatment, and the surface roughness Ra after sand blasting is 5-8 mm; s4, the Al wire and the Ti wire are thermally sprayed to the back target through electric arc equipment, and an AlTi target is obtained; and S5, the AlTi target material subjected to electric arc treatment is subjected to surface polishing treatment, and the surface roughness after polishing is smaller than or equal to Ra1.6 micrometers. The preparation method of the high-purity low-oxygen AlTi alloy target material has the advantages of being simple in technological operation, low in cost, high in target material purity and low in oxygen content.

Description

Technical Field

[0001] The invention relates to the field of sputtering coating, and more specifically, to a method for preparing a high-purity low-oxygen AlTi alloy target material. Background Art

[0002] During the coating deposition process, AlTi targets react with nitrogen to form TiAlN coatings, which have good toughness and oxidation resistance, greatly improving the cutting speed and cutting performance of drills, tools, indexable inserts and other tools and molds. AlTi targets are now also used in the photovoltaic industry as photovoltaic panels, which convert sunlight into electrical energy, usually outputting direct current and storing it in batteries. They are one of the most important components in home solar power generation.

[0003] How to prepare high-purity, low-oxygen AlTi alloy targets has become a key research direction in the industry.

[0004] Therefore, the present invention proposes a new solution to solve this problem. Summary of the invention

[0005] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a method for preparing a high-purity low-oxygen AlTi alloy target material, in which the AlTi alloy target material is prepared by arc thermal spraying, which has the advantages of simple process operation, low cost, high target purity and low oxygen content.

[0006] The above technical objectives of the present invention are achieved through the following technical solutions: A method for preparing a high-purity low-oxygen AlTi alloy target comprises the following steps:

[0007] S1: The raw materials are Al wire and Ti wire, and the diameter ratio of the Al wire to the Ti wire is 3:1;

[0008] S2: pickling the Al wire and the Ti wire with a cleaning agent, ultrasonically cleaning them with clean water for 30-60 minutes after pickling, drying them after cleaning, and installing them on the wire feeding reel of the vacuum arc equipment robot after drying;

[0009] S3: The back tube is subjected to a surface sandblasting treatment, and the surface roughness after sandblasting is Ra5-8mm;

[0010] S4: thermally spraying the Al wire and the Ti wire onto a back target using an arc device to obtain an AlTi target;

[0011] S5: Polish the AlTi target after arcing, and the surface roughness after polishing is ≤Ra1.6um

[0012] The present invention is further configured as follows: in step S1, the purity of the Al wire is ≥99.999%, the purity of the Ti wire is ≥99.8%, the diameter of the Al wire is 3±0.1 mm, and the diameter of the Ti wire is 1±0.1 mm.

[0013] The present invention is further configured as follows: in step S2, the cleaning agent is one of 5%-10% acetone solution, 5%-15% ethyl acetate solution, and banana water.

[0014] The present invention is further configured as follows: in step S2, the drying temperature is 50-80°C, and the drying time is 1-2h.

[0015] The present invention is further configured as follows: in step S3, the sandblasting grit is iron sand, silicon carbide sand or white corundum sand, and the grit mesh number is 20-40 meshes.

[0016] The present invention is further configured as follows: in step S3, the back tube rotation speed is 40-60r / min, the distance between the spray gun and the back tube surface is 100-150mm, the spray gun movement speed is 3-5mm / s, and the sandblasting pressure is 0.7-1.0Mpa.

[0017] The present invention is further configured as follows: in step S3, the back tube is made of 304 stainless steel or 316 stainless steel or Ti.

[0018] The present invention is further configured as follows: in step S4, the power of the arc spray gun is 10-18Kw, the rotation speed of the back tube is 20-60r / min, the distance between the spray gun and the outer surface of the back tube is 100-150mm, the moving speed of the spray gun is 80-120mm / min, the wire feeding speed of the Al wire is 80-100g / min, the wire feeding speed of the Ti wire is 40-50g / min, the thickness of the arc AlTi target is 12-28mm, and the ratio of the AlTi target is 95±2:5±1wt%.

[0019] The present invention is further configured as follows: in step S4, the arc spraying environment is a vacuum condition, and the vacuum degree is 10 -2 -10 -3 pa.

[0020] The present invention is further configured as follows: in step S5, the material of the polishing belt is aluminum oxide or diamond, and the mesh number of the polishing belt is 600-800 meshes.

[0021] In summary, the present invention has the following beneficial effects: the preparation method of the AlTi target material of the present invention has been proved by experiments that the relative density is ≥90%, the oxygen content is ≤100ppm, the purity is ≥3N6, and the grain size is ≤100um. The AlTi target material with good coating effect can be obtained by the above preparation method. By designing the purity and diameter of Al wire and Ti wire, and matching the wire feeding speed of Al wire and Ti wire in arc spraying, a target material with any AlTi ratio can be designed and manufactured. DETAILED DESCRIPTION

[0022] The present invention is described in detail below in conjunction with embodiments.

[0023] The present invention provides a method for preparing a high-purity low-oxygen AlTi alloy target, comprising the following steps:

[0024] S1: The raw materials used are Al wire with a purity of ≥99.999%, Ti wire with a purity of ≥99.8%, Al wire diameter of 3±0.1mm, Ti wire diameter of 1±0.1mm, and Al wire to Ti wire diameter ratio of 3:1;

[0025] S2: The Al wire and the Ti wire are cleaned with a cleaning agent of 5%-10% acetone solution, 5-15% ethyl acetate solution, or one of banana water, and then ultrasonically cleaned with clean water for 30-60 minutes after pickling, and then dried at a temperature of 50-80° C. for 1-2 hours. After drying, the wire is mounted on a wire feeding reel of a vacuum arc equipment manipulator;

[0026] S3: The back tube is subjected to sandblasting for surface roughening treatment. The sandblasting grit is iron sand, silicon carbide sand or white corundum sand, the grit mesh is 20-40 mesh, the back tube rotation speed is 40-60r / min, the distance between the spray gun and the back tube surface is 100-150mm. The spray gun movement speed is 3-5mm / s, the sandblasting pressure is 0.7-1.0Mpa, and the surface roughness after sandblasting is Ra5-8mm. The back tube material is 304 stainless steel or 316 stainless steel or Ti;

[0027] S4: using arc equipment to thermally spray the Al wire and Ti wire on the back target to obtain an AlTi target, the power of the arc spray gun is 10-18Kw, the rotation speed of the back tube is 20r / min-60r / min, the distance between the spray gun and the outer surface of the back tube is 100mm-150mm, the moving speed of the spray gun is 80mm / min-120mm / min, the wire feeding speed of the Al wire is 80-100g / min, the wire feeding speed of the Ti wire is 40-50g / min, the thickness of the arc AlTi target is 12-28mm, the ratio of the AlTi target is 95±2:5±1wt%, and the arc spraying environment is vacuum, and the vacuum degree is 10 -2-10 -3 pa;

[0028] S5: The AlTi target material after arcing is surface polished. The polishing belt is made of alumina or diamond. The mesh number of the polishing belt is 600-800. The surface roughness after polishing is ≤Ra1.6um.

[0029] The preparation method of the above AlTi target material has been proved by experiments that the relative density is ≥90%, the oxygen content is ≤100ppm, the purity is ≥3N6, and the grain size is ≤100um. The AlTi target material with good coating effect can be obtained by the above preparation method. By designing the purity and diameter of Al wire and Ti wire, and matching the wire feeding speed of Al wire and Ti wire in arc spraying, a target material with any AlTi ratio can be designed and manufactured.

[0030] The following is an example of a specific implementation:

[0031] Embodiment 1:

[0032] S1: The raw materials used are Al wire with a purity of 99.999% and Ti wire with a purity of 99.8%. The diameter of the Al wire is 3 mm and the diameter of the Ti wire is 1 mm.

[0033] S2: The Al wire and the Ti wire are cleaned with an 8% acetone solution as the cleaning agent, and then pickled and ultrasonically cleaned with clean water for 30 minutes. After cleaning, the wires are dried at a temperature of 80° C. for 1 hour. After drying, the wires are mounted on a wire feeding reel of a vacuum arc equipment robot.

[0034] S3: The back tube is subjected to a surface sandblasting roughening treatment, the sandblasting grit is iron sand, the grit mesh is 20 mesh, the back tube rotation speed is 40r / min, the distance between the spray gun and the back tube surface is 100mm, the spray gun movement speed is 3mm / s, the sandblasting pressure is 1.0Mpa, the surface roughness after sandblasting is Ra8mm, and the back tube material is 304 stainless steel.

[0035] S4: using arc equipment to thermally spray the Al wire and Ti wire onto the back target to obtain an AlTi target. The power of the arc spray gun is 10Kw, the rotation speed of the back tube is 20r / min, the distance between the spray gun and the outer surface of the back tube is 100mm, the moving speed of the spray gun is 80mm / min, the wire feeding speed of the Al wire is 80g / min, the wire feeding speed of the Ti wire is 40g / min, the thickness of the arc AlTi target is 12mm, the ratio of the AlTi target is 95.8:4.2wt%, and the arc spraying environment is vacuum, and the vacuum degree is 10 -2 pa.

[0036] S5: The AlTi target material after arcing is subjected to surface polishing treatment. The material of the polishing belt is alumina, the mesh number of the polishing belt is 800 mesh, and the surface roughness after polishing is Ra0.8um.

[0037] Embodiment 2:

[0038] S1: The raw materials used are Al wire with a purity of 99.9991% and Ti wire with a purity of 99.8%. The diameter of the Al wire is 2.9 mm and the diameter of the Ti wire is 0.9 mm.

[0039] S2: The Al wire and the Ti wire are cleaned with a 10% ethyl acetate solution as the cleaning agent, and then pickled and ultrasonically cleaned with clean water for 45 minutes. After cleaning, the wires are dried at a temperature of 65° C. for 1.5 hours. After drying, the wires are mounted on a wire feeding reel of a vacuum arc equipment robot.

[0040] S3: The back tube is subjected to a surface sandblasting treatment, wherein the sandblasting grit is silicon carbide sand, the grit mesh is 40 mesh, the back tube rotation speed is 50r / min, the distance between the spray gun and the back tube surface is 120mm, the spray gun movement speed is 5mm / s, the sandblasting pressure is 0.7Mpa, the surface roughness after sandblasting is Ra7mm, and the back tube material is 316 stainless steel.

[0041] S4: using arc equipment to thermally spray the Al wire and Ti wire onto the back target to obtain an AlTi target. The power of the arc spray gun is 15Kw, the rotation speed of the back tube is 40r / min, the distance between the spray gun and the outer surface of the back tube is 150mm, the moving speed of the spray gun is 100mm / min, the wire feeding speed of the Al wire is 100g / min, the wire feeding speed of the Ti wire is 50g / min, the thickness of the arc AlTi target is 20mm, the ratio of the AlTi target is 95.3:4.7wt%, and the arc spraying environment is vacuum, and the vacuum degree is 10 -3 pa.

[0042] S5: The AlTi target material after arcing is surface polished. The polishing belt is made of alumina, the mesh number of the polishing belt is 600 mesh, and the surface roughness after polishing is Ra1.6um.

[0043] Embodiment 3:

[0044] S1: The raw materials used are Al wire with a purity of 99.999% and Ti wire with a purity of 99.9%. The diameter of the Al wire is 3.1 mm and the diameter of the Ti wire is 1.1 mm.

[0045] S2: The Al wire and the Ti wire are cleaned with banana water as the cleaning agent, and then pickled and ultrasonically cleaned with clean water for 30-60 minutes. After cleaning, the wires are dried at a temperature of 50° C. for 2 hours. After drying, the wires are mounted on the wire feeding reel of the vacuum arc equipment robot.

[0046] S3: The back tube is subjected to a surface sandblasting roughening treatment, the sandblasting grit is white corundum sand, the grit mesh is 24 mesh, the back tube rotation speed is 60r / min, the distance between the spray gun and the back tube surface is 150mm. The spray gun movement speed is 4mm / s, the sandblasting pressure is 0.8Mpa, the surface roughness after sandblasting is Ra5mm, and the back tube material is Ti.

[0047] S4: using arc equipment to thermally spray the Al wire and Ti wire onto the back target to obtain an AlTi target. The power of the arc spray gun is 18Kw, the rotation speed of the back tube is 60r / min, the distance between the spray gun and the outer surface of the back tube is 120mm, the moving speed of the spray gun is 120mm / min, the wire feeding speed of the Al wire is 90g / min, the wire feeding speed of the Ti wire is 45g / min, the thickness of the arc AlTi target is 28mm, the ratio of the AlTi target is 94.3:5.7wt%, and the arc spraying environment is vacuum, and the vacuum degree is 10 -2 pa.

[0048] S5: The AlTi target material after arcing is subjected to surface polishing treatment. The polishing belt is made of diamond, the mesh number of the polishing belt is 700 mesh, and the surface roughness after polishing is Ra1.1um.

[0049] Comparative Example 1

[0050] S1: Selecting Al ingots with a purity of 99.999% and Ti ingots with a purity of 99.8% as raw materials, adding 50% of the Al ingots into a medium frequency melting furnace, adding the Ti ingots after the Al ingots are dissolved, the melting temperature is 1150°C, and after the Ti ingots are melted, the remaining Al ingots are put into the melting furnace, and cast to prepare AlTi10 alloy ingots;

[0051] S2: putting the alloy ingot and the Al ingot into a medium frequency induction furnace according to the finished product ratio of 95:5wt%, with a melting temperature of 1050°C and a melting time of 30-40min;

[0052] S3: The back tube is subjected to sandblasting for surface roughening. The sandblasting grit is iron sand, the grit mesh is 20 mesh, the back tube rotation speed is 40r / min, the distance between the spray gun and the back tube surface is 100mm. The spray gun movement speed is 3mm / s, the sandblasting pressure is 1.0Mpa, and the surface roughness after sandblasting is Ra8mm. The back tube is made of 304 stainless steel.

[0053] S4: arc treatment of the back tube, using NiAl wire in a ratio of 95:5wt%, a power of 20kw, a moving speed of the arc spray gun of 100mm / min, a distance of the arc spray gun from the back tube of 100mm, and a surface roughness of the back tube after arcing of Ra12um.

[0054] S5: heat the back tube after the sandblasting arc at a temperature of 600°C, cast the AlTi alloy solution on the 304 back tube at a casting temperature of 1100°C, and naturally cool to room temperature for 8 hours after casting;

[0055] S6: AlTi target surface is machined to the size required by the customer.

[0056] The product performance of Examples 1, 2, 3 and Comparative Example 1 was compared to obtain the data in Table 1.

[0057] Table 1: Comparison of key parameters and product performance

[0058]

[0059] Compared with the prior art, the AlTi target prepared by the present invention has the following characteristics:

[0060] (1) Compared with traditional fused casting targets, the process is simpler, safer, 70% lower in cost than fused casting, the oxygen content is very low, the surface and internal quality of the target is better, and the target with a specific proportion can be customized according to customer needs;

[0061] (2) The arc spraying target material has stable dimensions. The cast target material has serious Ti element segregation due to the large difference in the melting point of AlTi, and the casting temperature is high, resulting in serious deformation of the back tube and low yield.

[0062] The above is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above embodiments. All technical solutions under the concept of the present invention belong to the protection scope of the present invention. It should be pointed out that for ordinary technicians in this technical field, some improvements and modifications without departing from the principle of the present invention should also be regarded as the protection scope of the present invention.

Claims

1. A method for preparing a high-purity low-oxygen AlTi alloy target, characterized in that: The following steps are involved: S1: The raw materials are Al wire and Ti wire, and the diameter ratio of the Al wire to the Ti wire is 3:1; S2: pickling the Al wire and the Ti wire with a cleaning agent, ultrasonically cleaning them with clean water for 30-60 minutes after pickling, drying them after cleaning, and installing them on the wire feeding reel of the vacuum arc equipment robot after drying; S3: The back tube is subjected to surface sandblasting and roughening treatment, and the surface roughness after sandblasting is Ra5-8mm; S4: thermally spraying the Al wire and the Ti wire onto a back target using an arc device to obtain an AlTi target; S5: The AlTi target material after arcing is subjected to surface polishing treatment, and the surface roughness after polishing is ≤Ra1.6um.

2. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1, characterized in that: In step S1, the purity of the Al wire is ≥99.999%, the purity of the Ti wire is ≥99.8%, the diameter of the Al wire is 3±0.1 mm, and the diameter of the Ti wire is 1±0.1 mm.

3. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1, characterized in that: In step S2, the cleaning agent is one of 5%-10% acetone solution, 5%-15% ethyl acetate solution, and banana water.

4. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 3, characterized in that: In step S2, the drying temperature is 50-80°C and the drying time is 1-2h.

5. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1, characterized in that: In step S3, the sandblasting grit is iron sand, silicon carbide sand or white corundum sand, and the grit mesh number is 20-40 meshes.

6. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1 or 5, characterized in that: In step S3, the back tube rotation speed is 40-60r / min, the distance between the spray gun and the back tube surface is 100-150mm, the spray gun movement speed is 3-5mm / s, and the sandblasting pressure is 0.7-1.0Mpa.

7. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1 or 5, characterized in that: In step S3, the back tube is made of 304 stainless steel, 316 stainless steel or Ti.

8. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1, characterized in that: In step S4, the power of the arc spray gun is 10-18Kw, the rotation speed of the back tube is 20-60r / min, the distance between the spray gun and the outer surface of the back tube is 100-150mm, the moving speed of the spray gun is 80-120mm / min, the wire feeding speed of the Al wire is 80-100g / min, the wire feeding speed of the Ti wire is 40-50g / min, the thickness of the arc AlTi target is 12-28mm, and the ratio of AlTi target is 95±2:5±1wt%.

9. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 8, characterized in that: In step S4, the arc spraying environment is a vacuum state, and the vacuum degree is 10 -2 -10 -3 pa.

10. The method for preparing a high-purity low-oxygen AlTi alloy target according to claim 1, characterized in that: In step S5, the polishing belt is made of aluminum oxide or diamond, and the mesh number of the polishing belt is 600-800 meshes.

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