A method for preparing aluminum-titanium target material by combining rolling and warm pressing of aluminum-titanium waste target material

The problem of low utilization rate of aluminum-titanium targets is solved by combining the stacking and warm pressing of aluminum-titanium waste targets, and efficient and environmentally friendly reuse is achieved. The welding rate is high and it is suitable for high-power sputtering coating.

CN119657634BActive Publication Date: 2025-09-05XIANGTAN UNIV
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Patent Information

Application Number
CN202411920258.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-25
Publication Date
2025-09-05
Estimated Expiration
2044-12-25

AI Technical Summary

Technical Problem

In the existing technology, the utilization rate of aluminum-titanium targets is low, the recycling method is cumbersome, costly and causes serious environmental pollution, making it difficult to achieve efficient and environmentally friendly reuse.

Method used

The method of combining aluminum-titanium waste target material lamination and warm pressing is adopted. Aluminum powder is sprayed on the surface of the target material as a soft intermediate layer, and pre-lamination and warm pressing treatment is performed to expand the diffusion connection area and improve the welding rate.

Benefits of technology

It realizes efficient and environmentally friendly recycling of aluminum-titanium targets with high welding rate, is suitable for high-power sputtering coating, and reduces environmental pollution and production costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a method for preparing an aluminum-titanium target by combining aluminum-titanium waste target rolling with warm pressing, which belongs to the field of powder metallurgy technology. The preparation method is as follows: the aluminum-titanium waste target is pretreated to obtain an aluminum-titanium target semi-finished product, N sheets of aluminum-titanium target semi-finished products are taken, and a slurry containing aluminum powder is sprayed on the surface of N sheets or N-1 sheets of aluminum-titanium target semi-finished products. After spraying is completed, the N sheets of aluminum-titanium target semi-finished products are stacked to obtain a composite plate, the composite plate is rolled to obtain a composite target, and then the composite target is subjected to warm pressing to obtain an aluminum-titanium target. The preparation method of the present invention, the warm pressing process allows sufficient diffusion between the targets, and the pre-rolling process reduces the effect of surface flatness on diffusion, and aluminum powder, as a soft intermediate layer, plays a good buffering and caulking effect, which is conducive to promoting the diffusion, so that the target welding rate is> 95% in the preferred embodiment. The preparation method of the present invention improves the utilization rate of the target, reduces the production cost of the target, and realizes the recycling of the target.
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Description

Technical Field

[0001] The invention relates to a method for preparing an aluminum-titanium target material by utilizing aluminum-titanium waste target material stacking and warm pressing, and belongs to the technical field of aluminum-titanium target material preparation. Background Art

[0002] Hard-coated targets are primarily used in machining applications such as cutting tools and wear-resistant parts. Physical vapor deposition (PVD) can effectively improve cutting performance and extend tool life. Commonly used hard-coated targets include aluminum-titanium, aluminum-chromium, and titanium-silicon. Aluminum-titanium targets are deposited on workpiece surfaces using physical vapor deposition (PVD) in a nitrogen atmosphere. This hard coating has promising application prospects in the machining industry due to its excellent wear and heat resistance. Currently, aluminum-titanium targets are primarily produced through powder metallurgy.

[0003] In actual production, most target materials cannot be fully utilized. During use, a reverse sputtering layer will be generated on the surface of the target, forming a wavy appearance. When the sputtering depth exceeds the maximum limit, continued use is likely to penetrate the target. Therefore, when the sputtering target material is consumed to a certain extent, the thin target material is usually discarded, resulting in a large amount of waste target material generated during the production and use of the target material. Generally speaking, the part of the target material that can be effectively utilized is only 30% to 40% of its original weight. This low utilization rate is undoubtedly a huge waste for the target material, which is difficult to produce and expensive. If the remaining discarded aluminum-titanium targets can be recycled and reused at low cost and high efficiency, it will have great economic value.

[0004] Currently, most methods for recycling waste targets involve alkali washing, pickling, water washing, smelting, casting, and then processing and binding the waste targets before returning them to production. However, due to the large difference in melting points between titanium and aluminum in titanium-aluminum targets, it is difficult to prepare uniform aluminum-titanium targets during smelting. Furthermore, such methods are cumbersome, consume large amounts of materials and energy, and are costly. Furthermore, the large amount of waste liquid generated during the pickling and alkali washing of the waste targets causes environmental pollution. Therefore, the development of a new, efficient, and environmentally friendly aluminum-titanium target recycling method without separating and smelting the targets is of great significance for both target manufacturing and carbide tool cutting. Summary of the Invention

[0005] In response to the shortcomings of the existing technology, the present invention provides a method for preparing aluminum-titanium targets by combining rolling and warm pressing of waste aluminum-titanium targets. The present invention prepares reusable finished targets by recycling waste targets, thereby solving the problem of low utilization rate of sputtering targets during use. Moreover, the method of the present invention does not require the separation and smelting of the targets, and can achieve the recycling of aluminum-titanium targets only by rolling and warm pressing. The method is efficient, environmentally friendly, and has a simple preparation process.

[0006] In order to achieve the above purpose, the present invention adopts the following technical solutions:

[0007] The present invention provides a method for preparing an aluminum-titanium target material by combining rolling and warm pressing of waste aluminum-titanium target materials. The waste aluminum-titanium target materials are pretreated to obtain a semi-finished aluminum-titanium target. N (or N-1) pieces of the semi-finished aluminum-titanium target materials are sprayed with a slurry containing aluminum powder. After spraying, the N pieces of the semi-finished aluminum-titanium target materials are stacked to obtain a composite plate. The composite plates are then rolled to obtain a composite target material. The composite target material is then warm pressed to obtain the aluminum-titanium target material.

[0008] The preparation method of the present invention spreads a layer of aluminum powder on the surface of the aluminum-titanium target semi-finished product. The aluminum powder serves as a soft intermediate layer transition and plays a good buffering and filling role. Then, rolling is performed at a certain temperature to cause plastic deformation of the relative contact surfaces of the aluminum-titanium target semi-finished product, greatly increasing the contact area of ​​the connected interface and expanding the range of the diffusion connection zone. Finally, the prepared aluminum-titanium target has a high welding rate.

[0009] In the present invention, the aluminum-titanium waste target material used is the aluminum-titanium waste target material that has become thinner and cannot be further used after coating application.

[0010] In the present invention, any aluminum-titanium waste target with any aluminum-titanium ratio is applicable. The following preferred atomic ratios are for commonly used aluminum-titanium waste targets.

[0011] In a preferred embodiment, the aluminum-titanium waste target material has an atomic ratio of Al:Ti = 40-70:30-60.

[0012] In a preferred embodiment, the pretreatment is to sequentially mill and flatten the aluminum-titanium waste target material.

[0013] In the actual operation process, the aluminum-titanium waste target material is ultrasonically cleaned for 10 to 15 minutes, foreign matter on the surface of the waste target after coating is removed by milling, and the surface of the target material is flattened to obtain an aluminum-titanium target semi-finished product; the surface flattening treatment is to machine grind the surface of the aluminum-titanium target semi-finished product, and then ultrasonically clean it with acetone for about 15 minutes after flattening to obtain the aluminum-titanium target semi-finished product.

[0014] In a preferred embodiment, the thickness of the semi-finished aluminum-titanium target is 3-4 mm. The inventors have found that controlling the thickness of the semi-finished aluminum-titanium target within this range results in a high yield rate and high quality of the resulting aluminum-titanium target. If the thickness is too thin, the yield rate is reduced, while if the thickness is too thick, impurity particles from the waste target may be introduced, affecting the quality of the finished target.

[0015] In a preferred embodiment, the surface roughness of the aluminum-titanium target semi-finished product is 2.5-6.5 μm. The inventors have found that controlling the surface roughness of the aluminum-titanium target semi-finished product within this range maximizes the final weldability. Excessive roughness may create numerous voids at the bonding interface, hindering the warm-press diffusion process.

[0016] In a preferred embodiment, the flatness of the semi-finished aluminum-titanium target is ≤0.1 mm.

[0017] In a preferred embodiment, the particle size D of the aluminum powder is 50 The particle size of aluminum powder is controlled within this range, and the welding rate of all products is the highest. If the particle size is too small, the gap filling effect in some areas may not be obvious, which is not conducive to the subsequent temperature and pressure diffusion. If the particle size is too large, it may make stacking difficult and affect the bonding between the target semi-finished products.

[0018] Preferably, the aluminum powder-containing slurry is obtained by wet ball milling the aluminum powder.

[0019] Further preferably, during the wet ball milling, zirconia balls are used, anhydrous ethanol is used as the grinding medium, the powder-ball mass ratio is 1:(2-4), the ball milling speed is 200-500 r / min, and the ball milling time is 15-100 min.

[0020] The preferred solution is to take N pieces of aluminum-titanium target semi-finished products, spray a slurry containing aluminum powder on the surface of N or N-1 pieces of aluminum-titanium target semi-finished products, and after spraying is completed, stack the N pieces of aluminum-titanium target semi-finished products to obtain a composite plate, and control the N-1 interfaces formed in the composite plate to contain an aluminum powder layer with a thickness of 0.25~0.5mm.

[0021] In the present invention, except for ensuring that the surfaces of the aluminum-titanium target semi-finished products on the two outer sides of the composite plate are not sprayed, the spraying method for other surfaces is not limited. It is only necessary to control that after stacking, the contact surface of any two aluminum-titanium target semi-finished products, that is, the interface of the composite plate, contains an aluminum powder layer with a thickness of 0.25 to 0.5 mm. The thickness of the aluminum powder layer is controlled within the range of the present invention, and the final welding rate is the highest.

[0022] In a preferred embodiment, N is 3 to 5, preferably 4.

[0023] In a preferred embodiment, the number of passes of the lap rolling is 1 to 2.

[0024] Furthermore, the total reduction during the rolling process is preferably 3% to 6% of the total thickness of the aluminum-titanium target semi-finished product. Keeping the reduction within this range maximizes the weldability and quality of the resulting aluminum-titanium target. Excessive reduction can cause internal cracks.

[0025] In a preferred embodiment, the warm pressing is carried out under the protection of an argon atmosphere, the temperature of the warm pressing is 400-500°C, preferably 450-500°C, the time of the warm pressing is 2-10 hours, preferably 5-10 hours; the heating rate is 3-5°C / min, preferably 5°C / min; the loading pressure is 30-50 MPa, preferably 40-50 MPa,

[0026] By controlling the temperature of the warm pressing within the range of the present invention and fully keeping it warm, sufficient diffusion can be achieved, and finally a finished target material with high welding rate and good quality can be obtained. If the temperature of the warm pressing is too low, it is not conducive to sufficient diffusion during warm pressing. If the temperature is too high, the composite target material will produce excessive thermal expansion, and the increase in internal stress will also increase its crack tendency. If the pressure is too low, it is not conducive to close contact of the connection interface and reduces the efficiency of diffusion. If the pressure is too high, it may cause excessive extrusion and affect the quality of the final finished target material.

[0027] The welding rate of the connection surfaces between the aluminum-titanium target layers prepared by the above method is greater than 95% in a preferred embodiment.

[0028] Compared with the prior art, the advantages of the present invention are:

[0029] (1) The recycling and reuse method of the aluminum-titanium target material of the present invention is based on a method of pre-rolling and warm pressing of the same type of target material. Under this method, the preparation cycle of the target material is short, the recycling rate is high, and the reused target material with excellent performance can be obtained, and environmental pollution is greatly reduced;

[0030] (2) A layer of aluminum powder is applied to the surface of the semi-finished aluminum-titanium target material in the present invention. The aluminum powder acts as a soft intermediate layer transition, plays a good role in buffering and filling gaps, and is beneficial to promoting the diffusion between atoms during the temperature pressing process and improving the welding rate of the target material.

[0031] (3) The warm pressing process of the present invention utilizes the diffusion principle to form a technology that combines pre-rolling and warm pressing diffusion. No matter how rigorously the material surface is processed, when two interfaces are placed together, the surfaces will only exist in the form of point contact, and will be randomly distributed on the connected surfaces. Therefore, due to the influence of surface flatness, there will always be a certain gap between the interfaces. The present invention uses a small amount of pre-rolling to cause plastic deformation of the relative contact surfaces at a certain temperature, greatly increasing the contact area of ​​the connected interfaces and expanding the range of the diffusion connection zone, which is conducive to promoting the diffusion process;

[0032] (4) The aluminum-titanium target material of the present invention has a high welding rate, and the final welding rate obtained is >95% in the preferred embodiment. It is suitable for high-power, high-efficiency sputtering coating targets and has great prospects for actual production applications. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In order to explain the present invention more clearly, the specific implementation methods of the present invention will be further described in detail below, and specific embodiments of the present invention are given in conjunction with the accompanying drawings.

[0034] Figure 1 This is a schematic diagram of the structure of the temperature pressing equipment of the present invention; wherein 1-furnace body, 2-heating element, 3-workpiece, 4-induction coil;

[0035] Figure 2 This is a process flow chart for preparing aluminum-titanium targets according to the present invention;

[0036] Figure 3 This is a 100x optical microscope image of the diffusion joint interface of the aluminum-titanium target in Example 1;

[0037] Figure 4 The surface SEM of the sample after target coating in Example 1;

[0038] Figure 5 This is a physical picture of a single piece of aluminum-titanium waste target;

[0039] Figure 6 This is a photo of the finished product of the aluminum-titanium target prepared in Example 1. DETAILED DESCRIPTION

[0040] The following will further illustrate the research content of the present invention with reference to embodiments, and provide a clear and complete description of the technical solution of the present invention. However, the embodiments described are only part of the embodiments of the present invention, rather than all of the embodiments. The purpose of providing the embodiments is to make the content disclosed in the present invention more comprehensive.

[0041] See Figure 1 The present invention provides a temperature-pressing device comprising a furnace body 1, internally provided with an induction coil 4 and a heating element 2, wherein the heating element is disposed on the inner wall of the furnace body. An argon inlet valve and an argon outlet valve are provided above the furnace body, respectively. The inlet is connected to an argon cylinder, and the outlet is connected to water to prevent air backflow. A workpiece 3 is positioned between upper and lower pressing heads and surrounded by the induction coil.

[0042] Example 1:

[0043] The embodiment of the present invention discloses a method for recycling aluminum-titanium targets, which specifically includes the following steps:

[0044] (1) Prepare 4 pieces of Al after coating 0.7 Ti 0.3The waste targets were milled to 3-4 mm each to obtain aluminum-titanium target semi-finished products. The semi-finished products weighed 247.5 g, 251.6 g, 248.2 g, and 241.1 g, respectively, for a total mass of 988.4 g. The aluminum-titanium target semi-finished products were ultrasonically cleaned in acetone for 15 minutes and mechanically polished on both sides to a surface roughness of Ra = 2.5 μm and a flatness of less than or equal to 0.1 mm. They were then ultrasonically cleaned again for 15 minutes.

[0045] (2) Prepare particle size D 50 = 10 μm aluminum powder is evenly distributed on the surface of the aluminum-titanium target semi-finished product by spraying powder slurry;

[0046] (3) Four semi-finished products covered with aluminum powder are stacked together in sequence, and the N-1 interfaces formed by the composite are controlled to contain an aluminum powder layer of 0.25~0.5mm thick. They are pre-stacked in a two-wheel rolling mill, and the total reduction during the stacking is about 5% of the total thickness of the aluminum-titanium target semi-finished product;

[0047] (4) Place the semi-finished products after pre-stacked rolling into the warm pressing equipment, and use the vacuum pump to evacuate the furnace so that the relative vacuum degree in the furnace is less than or equal to 1×10 -2 pa, then argon was introduced into the furnace for 10 min, and the vacuum and ventilation treatment was repeated three times;

[0048] (5) After the purge is completed, maintain the argon atmosphere and use the heating element to raise the furnace temperature to 500℃ at a heating rate of 5℃ / min and keep it warm for 10 hours. At the same time, the loading pressure of the upper and lower pressure heads is maintained at 50Mpa during the insulation stage. After the insulation and pressure are completed, stop heating and cool the furnace to room temperature;

[0049] (6) The target material after diffusion is taken out, and the surface welding rate is measured by ultrasonic testing (UT) to be 97.5%. After milling on both sides and ultrasonic cleaning, the reusable aluminum-titanium regenerated target material is obtained. The mass of the finished target is measured to be 864.2g, and the yield rate is 87.4%;

[0050] The target material bonding interface after the diffusion of this embodiment is as follows Figure 3 As shown in Figure 2, an intermediate diffusion layer is formed at the connection interface, and there is no obvious gap in the joint, indicating that the connection is good.

[0051] The prepared target was coated on a cemented carbide WC substrate by cathode arc evaporation (CAE) technology. The SEM image of the coating surface was as follows: Figure 4 As shown in the figure, the coating has no obvious defects except for a small amount of droplets and pits after cathode arc evaporation deposition, indicating that the finished target material prepared by this invention is of good quality.

[0052] Example 2:

[0053] The embodiment of the present invention discloses a method for recycling aluminum-titanium targets, which specifically includes the following steps:

[0054] (1) Prepare 4 pieces of Al after coating 0.5 Ti 0.5 The waste targets were milled to 3-4 mm each to obtain aluminum-titanium target semi-finished products. The semi-finished products weighed 253.4 g, 248.9 g, 255.6 g, and 251.3 g, respectively, for a total mass of 1009.2 g. The aluminum-titanium target semi-finished products were ultrasonically cleaned in acetone for 15 minutes and mechanically polished on both sides to a surface roughness of Ra = 4 μm and a flatness of less than or equal to 0.1 mm. They were then ultrasonically cleaned again for 15 minutes.

[0055] (2) Prepare particle size D 50 = 10 μm aluminum powder is evenly distributed on the surface of the aluminum-titanium target semi-finished product by spraying powder slurry;

[0056] (3) Four semi-finished products covered with aluminum powder are stacked together in sequence, and the three interfaces formed by the composite are controlled to contain an aluminum powder layer of 0.25~0.5mm thick. They are pre-stacked in a two-wheel rolling mill, and the total reduction during the stacking is about 5% of the total thickness of the aluminum-titanium target semi-finished product;

[0057] (4) Place the semi-finished products after pre-stacked rolling into the warm pressing equipment, and use the vacuum pump to evacuate the furnace so that the relative vacuum degree in the furnace is less than or equal to 1×10 -2 pa, then argon was introduced into the furnace for 10 min, and the vacuum and ventilation treatment was repeated three times;

[0058] (5) After the purge is completed, maintain the argon atmosphere and use the heating element to raise the furnace temperature to 500℃ at a heating rate of 5℃ / min and keep it warm for 10 hours. At the same time, the loading pressure of the upper and lower pressure heads is maintained at 50Mpa during the insulation stage. After the insulation and pressure are completed, stop heating and cool the furnace to room temperature;

[0059] (6) The target material after diffusion is taken out, and the surface welding rate is measured by ultrasonic testing (UT) to be 96.3%. After milling on both sides and ultrasonic cleaning, the reusable aluminum-titanium recycled target material is obtained. The mass of the finished target is measured to be 874.2g, and the yield rate is 86.6%.

[0060] Example 3:

[0061] The embodiment of the present invention discloses a method for recovering an aluminum-titanium target, which specifically comprises the following steps:

[0062] (1) Prepare 4 pieces of Al after coating 0.4 Ti 0.6The waste targets were milled to 3-4 mm each to obtain semi-finished aluminum-titanium targets. The semi-finished products weighed 258.6 g, 257.1 g, 263.5 g, and 262.8 g, respectively, for a total mass of 1042 g. The semi-finished aluminum-titanium targets were ultrasonically cleaned in acetone for 15 minutes and mechanically polished on both sides to a surface roughness of Ra = 5.5 μm and a flatness of less than or equal to 0.1 mm. They were then ultrasonically cleaned again for 15 minutes.

[0063] (2) Prepare particle size D 50 = 10 μm aluminum powder, the aluminum powder is evenly distributed on the surface of the aluminum-titanium target semi-finished product by spraying powder slurry;

[0064] (3) Four semi-finished products covered with aluminum powder are stacked together in sequence, and the three interfaces formed by the composite are controlled to contain an aluminum powder layer of 0.25~0.5mm thick. They are pre-stacked in a two-wheel rolling mill, and the total reduction during the stacking is 5% of the total thickness of the aluminum-titanium target semi-finished product;

[0065] (4) Place the semi-finished products after pre-stacked rolling into the warm pressing equipment, and use the vacuum pump to evacuate the furnace so that the relative vacuum degree in the furnace is less than or equal to 1×10 -2 pa, then argon was introduced into the furnace for 10 min, and the vacuum and ventilation treatment was repeated three times;

[0066] (5) After the purge is completed, maintain the argon atmosphere and use the heating element to raise the furnace temperature to 500℃ at a heating rate of 5℃ / min and keep it warm for 10 hours. At the same time, the loading pressure of the upper and lower pressure heads is maintained at 50Mpa during the insulation stage. After the insulation and pressure are completed, stop heating and cool the furnace to room temperature;

[0067] (6) The target material after diffusion is taken out, and the surface welding rate is measured by ultrasonic testing (UT) to be 95.2%. After milling on both sides and ultrasonic cleaning, the reusable aluminum-titanium recycled target material is obtained. The mass of the finished target is measured to be 881.6 g, and the yield rate is 84.6%.

[0068] Example 4:

[0069] 4 pieces of Al prepared for milling 0.7 Ti 0.3 The semi-finished target, each with a thickness of 3-4 mm, was ultrasonically cleaned, polished, and surface-painted with aluminum powder according to the method of Example 1, and then pre-laminated in a two-wheel rolling mill. After the lamination, the target was placed in a warm pressing device, and the furnace temperature was raised to 400° C. at a heating rate of 5° C. / min and kept warm for 10 hours by a heating element. At the same time, the loading pressure of the upper and lower pressure heads was maintained at 50 MPa during the insulation stage. After the insulation and pressure holding period, the target was cooled to room temperature with the furnace. The welding rate of the connection interface was measured by ultrasonic testing (UT) to be 89.4%.

[0070] Example 5:

[0071] 4 pieces of Al prepared for milling 0.5 Ti 0.5 The semi-finished target, each with a thickness of 3-4 mm, was ultrasonically cleaned, polished, and surface-painted with aluminum powder according to the method of Example 2, and then pre-stacked in a two-wheel rolling mill. After the stacking was completed, it was placed in a warm pressing device, and the furnace temperature was raised to 500° C. at a heating rate of 5° C. / min and kept warm for 10 hours by a heating element. At the same time, the loading pressure of the upper and lower pressure heads was maintained at 30 MPa during the holding stage. After the holding and pressure holding were completed, the target was cooled to room temperature with the furnace. The welding rate of the connection interface was measured by ultrasonic testing (UT) to be 87.7%.

[0072] Example 6:

[0073] 4 pieces of Al prepared for milling 0.4 Ti 0.6 The semi-finished target, each with a thickness of 3-4 mm, was ultrasonically cleaned, polished, and surface-painted with aluminum powder according to the method of Example 3, and then pre-stacked in a two-wheel rolling mill. After the stacking was completed, it was placed in a warm pressing device, and the furnace temperature was raised to 500° C. at a heating rate of 5° C. / min and kept warm for 2 h. At the same time, the loading pressure of the upper and lower pressure heads was maintained at 50 MPa during the holding stage. After the holding and pressure holding were completed, the target was cooled to room temperature with the furnace. The welding rate of the connection interface was measured by ultrasonic testing (UT) to be 85.6%.

[0074] Comparative Example 1:

[0075] 4 pieces of Al prepared for milling 0.7 Ti 0.3 The semi-finished target, each with a thickness of 3-4 mm, was ultrasonically cleaned and polished according to the method of Example 1, and the surface was covered with titanium powder of the same particle size. It was pre-laminated in a two-wheel rolling mill. After the lamination, it was placed in a warm pressing device. The furnace temperature was raised to 500° C. at a heating rate of 5° C. / min and kept warm for 10 hours. At the same time, the loading pressure of the upper and lower pressure heads was maintained at 50 MPa during the insulation stage. After the insulation and pressure holding period, it was cooled to room temperature with the furnace. The welding rate of the connection interface was measured by ultrasonic flaw detection (UT) to be 63.3%.

[0076] Comparative Example 2:

[0077] 4 pieces of Al prepared for milling 0.7 Ti 0.3The semi-finished target has a thickness of 3-4 mm. It is ultrasonically cleaned and polished according to the method of Example 1, and the surface is no longer powdered. It is pre-stacked in a two-round rolling mill. After the stacking is completed, it is placed in a warm pressing device. The furnace temperature is raised to 500°C at a heating rate of 5°C / min and kept warm for 10 hours by a heating element. At the same time, the loading pressure of the upper and lower pressure heads is maintained at 50 MPa during the insulation stage. After the insulation and pressure are completed, it is cooled to room temperature with the furnace. The welding rate of the connection interface is measured by ultrasonic testing (UT) to be 56.8%.

[0078] For comparison of experimental results, the processes and results of Examples 1 to 6 and Comparative Examples 1 to 2 are shown in the table below, where the target welding rate is measured by ultrasonic testing (UT).

[0079]

[0080] It can be seen that in the method for preparing the aluminum-titanium target provided by the present invention, a reusable finished target with a high welding rate and excellent quality is efficiently prepared by cleaning the surface of the waste target and pre-stacking before warm pressing and diffusion. It can be seen from the performance results of the embodiment that the increase in the warm pressing temperature significantly makes the welding rate of the connection joint higher and the combination tighter. From the comparison of the embodiment and the comparative example, it can be seen that laying a diffusion intermediate layer on the surface of the aluminum-titanium semi-finished target material is also beneficial to improving the effect during warm pressing. When titanium powder is added, due to its hard and brittle nature, the target material is difficult to fit during the pre-stacking process and the deformation is large. When powder is not added, the gap at the connection interface is large, and it is difficult to produce interatomic diffusion during warm pressing. In summary, the effect of aluminum powder as a diffusion layer is significant.

[0081] The above description is only a specific embodiment of the present invention, and does not limit it. Those skilled in the art should understand that any modification, equivalent replacement or improvement of the technical solutions described in the aforementioned embodiments should be included in the scope of protection of the present invention.

Claims

1. A method for preparing aluminum-titanium targets by combining rolling and warm pressing of aluminum-titanium waste targets, characterized in that: The aluminum-titanium waste target materials are pretreated to obtain aluminum-titanium target semi-finished products, N pieces of aluminum-titanium target semi-finished products are taken, and a slurry containing aluminum powder is sprayed on the surface of N pieces or N-1 pieces of aluminum-titanium target semi-finished products. After the spraying is completed, the N pieces of aluminum-titanium target semi-finished products are stacked to obtain a composite plate, and the composite plates are rolled to obtain a composite target material, and then the composite target material is warm pressed to obtain the aluminum-titanium target material.

2. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1, characterized in that: In the aluminum-titanium waste target material, the atomic ratio of Al:Ti is 40-70:30-60.

3. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1, characterized in that: The pretreatment is to perform milling and flattening treatment on the aluminum-titanium waste target materials in sequence.

4. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1, characterized in that: The thickness of the aluminum-titanium target semi-finished product is 3-4 mm; The surface roughness of the aluminum-titanium target semi-finished product is 2.5-6.5 μm; The flatness of the aluminum-titanium target semi-finished product is ≤0.1 mm.

5. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1 or 4, characterized in that: The particle size D of the aluminum powder 50 5~50μm.

6. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1, characterized in that: The aluminum powder-containing slurry is obtained by wet ball milling the aluminum powder.

7. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 6, characterized in that: During the wet ball milling, zirconia balls are used, anhydrous ethanol is used as the grinding medium, the powder-ball mass ratio is 1:2-4, the ball milling speed is 200-500 r / min, and the ball milling time is 15-100 min.

8. The method for preparing aluminum-titanium targets by combining rolling and warm pressing of aluminum-titanium waste targets according to claim 1, characterized in that: Taking N semi-finished aluminum-titanium targets, spraying a slurry containing aluminum powder on the surfaces of N or N-1 semi-finished aluminum-titanium targets, and after the spraying is completed, stacking the N semi-finished aluminum-titanium targets to obtain a composite plate, and controlling the N-1 interfaces formed in the composite plate to contain an aluminum powder layer with a thickness of 0.25-0.5 mm; The N is 3~5.

9. The method for preparing an aluminum-titanium target by combining rolling and warm pressing of aluminum-titanium waste target materials according to claim 1, characterized in that: The number of passes of the lap rolling is 1 to 2 times; The total reduction of the stack rolling is 3% to 6% of the total thickness of the aluminum-titanium target semi-finished product.

10. The method for preparing aluminum-titanium targets by using aluminum-titanium waste targets by stacking and warm pressing according to claim 1, characterized in that: The warm pressing is carried out under the protection of an argon atmosphere, the temperature of the warm pressing is 400-500° C., the time of the warm pressing is 2-10 hours, the heating rate is 3-5° C. / min, and the loading pressure is 30-50 MPa.

Citation Information

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