A rare earth rotating target material and preparation method thereof
By adding aluminum sheets to the welding layer and combining it with heat treatment, the problems of desoldering and low utilization of rotating targets at high power density are solved, and efficient target utilization and oxidation protection are achieved.
Patent Information
- Application Number
- CN202211099977.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-09-07
- Publication Date
- 2025-09-19
- Estimated Expiration
- 2042-09-07
AI Technical Summary
Existing rotating targets for magnetron sputtering are prone to desoldering due to melting of solder under high power density, and the target utilization rate is low. In particular, rare earth targets are easily oxidized during the welding process, making welding difficult.
By adding aluminum sheets to the solder layer and combining it with a heat treatment process, the melting point of the solder is increased through segmented heat preservation treatment to form a high-melting-point alloy, ensuring that the solder does not melt at low temperatures and is evenly distributed.
The sputtering power density and utilization rate of the target material are improved, the oxidation risk of the rare earth target material is reduced, and low-temperature welding and efficient utilization are achieved.
Smart Images

Figure CN115533359B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical fields of magnetic materials, storage and electronic information, and in particular to a rare earth rotary target material and a preparation method thereof. Background Art
[0002] The rotating target for magnetron sputtering requires the target tube and the back tube to be welded together through a welding layer before use. The target sputtering power density is closely related to the quality of the welding layer. In the existing technology, indium is usually used as the solder. On the one hand, since the melting point of indium is only 156.6°C, the use of a higher power density will cause the solder to melt, resulting in target desoldering; on the other hand, the target becomes thinner in the later stage of sputtering, and the melting of the solder is an important factor restricting the utilization rate of the target; the use of solders with higher melting points such as tin and indium tin alloy can increase the sputtering power density, but the high welding temperature can easily lead to oxidation of the chemically active rare earth target during the welding process, and it will also increase the difficulty of target welding. Summary of the Invention
[0003] Based on the above situation of the prior art, the purpose of the embodiment of the present invention is to provide a rare earth rotating target material and a preparation method thereof, by adding an aluminum sheet in the middle of the welding layer and combining it with a heat treatment process to increase the melting point of the solder, thereby achieving the purpose of increasing the sputtering power density and target utilization rate of the rare earth rotating target material.
[0004] To achieve the above object, according to one aspect of the present invention, a rare earth rotary target is provided, comprising a backing tube and at least one rare earth target tube welded to the outside of the backing tube;
[0005] The back tube and the rare earth target tube are welded via an intermediate welding layer, wherein the intermediate welding layer comprises a metal indium solder and at least one aluminum sheet disposed in the metal indium solder, wherein the aluminum content in the intermediate welding layer is 3-10 wt.%, and the back tube, the aluminum sheet and the rare earth target tube are concentric cylindrical structures.
[0006] Furthermore, the rare earth target tube includes any one of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium, and scandium.
[0007] Furthermore, the thickness of the single aluminum sheet is 0.05-0.15 mm.
[0008] According to another aspect of the present invention, there is provided a method for preparing the rare earth rotary target material as described in the first aspect of the present invention, comprising the steps of:
[0009] At a preset welding temperature, a metal indium solder is filled between the back tube and the rare earth target tube, and an aluminum sheet is placed in the metal indium solder; or an aluminum sheet is placed in the metal indium solder in advance, and then the metal indium solder with the aluminum sheet is filled between the back tube and the rare earth target tube, and the back tube and the rare earth target tube are welded to obtain a welded rare earth rotating target material;
[0010] performing heat treatment on the welded rare earth rotary target;
[0011] The rare earth rotary target after heat treatment is cooled to room temperature and cleaned.
[0012] Furthermore, it also includes:
[0013] Prior to filling, the aluminum sheet is pre-coated with a layer of metallic indium solder.
[0014] Furthermore, the preset welding temperature is 190-230°C.
[0015] Furthermore, the heat treatment comprises the following steps:
[0016] Cooling the welded rare earth rotary target to room temperature and then cleaning it;
[0017] The cleaned rare earth rotary target is placed in a vacuum heat treatment furnace and the vacuum is pumped to 10 -3 Below Pa;
[0018] The rare earth rotary target is directly heat-treated or heat-treated after being filled with inert gas. The heat treatment temperature is 140° C. to 640° C., and the heat treatment time is 0.5 to 50 hours.
[0019] Furthermore, the heat treatment is a segmented heat preservation treatment, comprising:
[0020] Heat treatment at 140°C for 0.5-1h;
[0021] Heat treatment at 157°C for 1-3 hours;
[0022] Heat treatment at 200℃ for 1-3h;
[0023] Heat treatment at 250℃ for 1-3h;
[0024] Heat treatment at 300℃ for 1-3h;
[0025] Heat treatment at 350℃ for 1-5h;
[0026] Heat treatment at 400℃ for 1-5h;
[0027] Heat treatment at 450℃ for 1-5h;
[0028] Heat treatment at 500℃ for 1-5h;
[0029] Heat treatment at 550℃ for 1-5h;
[0030] Heat treatment at 600℃ for 1-5h;
[0031] Heat treatment at 630℃ for 1-6h.
[0032] In summary, an embodiment of the present invention provides a rare earth rotary target material and a preparation method thereof, wherein the rare earth rotary target material includes a back tube and at least one rare earth target tube welded to the outside of the back tube; the back tube and the rare earth target tube are welded via an intermediate welding layer, wherein the intermediate welding layer includes a metal indium solder and at least one aluminum sheet disposed in the metal indium solder, wherein the aluminum content in the intermediate welding layer is 3-10 wt.%, and the thickness of a single aluminum sheet is 0.05-0.15 mm. The back tube, the aluminum sheet, and the rare earth target tube are concentric cylindrical structures. The technical solution of the embodiment of the present invention focuses on target material welding, solder alloying, etc., and by adding an aluminum sheet in the middle of the welding layer and combining it with the heat treatment process, selecting a reasonable thickness can better control the melting point of the solder, reduce the segregation of solder components and reduce the contamination of the solder to the target material; adopting a segmented insulation treatment method for heat treatment, the solder is prevented from melting and flowing out, while ensuring the uniformity of the solder, and by gradually increasing the temperature, the solder indium and the like gradually form a high-melting-point alloy with aluminum, thereby improving the melting point of the alloy solder, achieving the purpose of increasing the sputtering power density and target utilization rate of the rare earth rotating target, realizing low-temperature welding and slowing down the oxidation of the rare earth target. BRIEF DESCRIPTION OF THE DRAWINGS
[0033] Figure 1 Schematic diagram of the overall structure of the rare earth rotary target provided by an embodiment of the present invention;
[0034] Figure 2 yes Figure 1 A cross-sectional view of the rare earth rotary target at c is shown;
[0035] Figure 3 This is a flow chart of a method for preparing a rare earth rotary target provided by an embodiment of the present invention. DETAILED DESCRIPTION
[0036] To make the objectives, technical solutions, and advantages of the present invention more clearly understood, the present invention will be further described in detail below in conjunction with specific embodiments and with reference to the accompanying drawings. It should be understood that these descriptions are merely exemplary and are not intended to limit the scope of the present invention. In addition, in the following description, descriptions of well-known structures and technologies are omitted to avoid unnecessary confusion of the concepts of the present invention.
[0037] It should be noted that, unless otherwise defined, the technical terms or scientific terms used in one or more embodiments of the present invention should have the usual meanings understood by people with ordinary skills in the field to which this disclosure belongs. The "first", "second" and similar words used in one or more embodiments of the present invention do not indicate any order, quantity or importance, but are only used to distinguish different components. "Include" or "comprise" and similar words mean that the elements or objects appearing before the word include the elements or objects listed after the word and their equivalents, without excluding other elements or objects. "Connect" or "connected" and similar words are not limited to physical or mechanical connections, but may include electrical connections, whether direct or indirect. "Up", "down", "left", "right" and the like are only used to indicate relative positional relationships. When the absolute position of the object being described changes, the relative positional relationship may also change accordingly.
[0038] The technical solution of the present invention is described in detail below with reference to the accompanying drawings. An embodiment of the present invention provides a rare earth rotating target material, Figure 1 Schematic diagram of the overall structure of the rare earth rotary target is shown in FIG. , wherein the rare earth rotary target comprises a backing tube 1 and at least one rare earth target tube welded to the outside of the backing tube. Figure 1 The following diagram illustrates four sections of rare earth target tubes, including target tube A1, target tube A2, target tube A3, and target tube A4. The target tubes are joined together, with a certain gap left at the joints based on the expansion coefficient.
[0039] Figure 2 Shown in Figure 1 The cross-sectional view of the rare earth rotary target at c is as follows: Figure 2 As shown, a backing tube 1 and a rare earth target tube A are welded together via an intermediate welding layer. The intermediate welding layer comprises a metallic indium solder 3 and at least one aluminum sheet 2 disposed within the metallic indium solder. The aluminum content of the intermediate welding layer is 3-10 wt.%. The backing tube 1, the aluminum sheet 2, and the rare earth target tube A form concentric cylindrical structures. The rare earth target tube A comprises any one of lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), terbium (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), lutetium (Lu), scandium (Sc), and yttrium (Y). The thickness of the single aluminum sheet 2 is 0.05-0.15 mm. The selection of this thickness can better control the melting point of the solder and make the composition more uniform. If the thickness is too large, the alloying time will be long and the composition deviation will be large. If the thickness is too small, it will easily lead to a high target material composition in the solder layer and contaminate the target material.
[0040] The embodiment of the present invention further provides a method for preparing a rare earth rotating target material, wherein the rare earth rotating target material is the rare earth selective target material involved in the above embodiment of the present invention. Figure 3 , which shows a flow chart of a method for preparing the rare earth rotary target, and which comprises the following steps:
[0041] S1. At a preset welding temperature, for example, 190°C to 230°C, fill the space between the back tube and the rare earth target tube with metal indium solder and place an aluminum sheet in the metal indium solder; or, after pre-placing the aluminum sheet in the metal indium solder, fill the space between the back tube and the rare earth target tube with the metal indium solder and the aluminum sheet, and weld the back tube and the rare earth target tube to obtain a welded rare earth rotating target. To improve welding quality, a layer of metal indium solder may be pre-coated on the aluminum sheet before filling.
[0042] S2. Heat treating the welded rare earth rotary target; the heat treatment comprises the following steps:
[0043] Cooling the welded rare earth rotary target to room temperature and then cleaning it;
[0044] The cleaned rare earth rotary target is placed in a vacuum heat treatment furnace and the vacuum is pumped to 10 -3 Below Pa;
[0045] The rare earth rotary target is directly heat-treated or heat-treated after being filled with inert gas, with the heat treatment temperature being 140°C to 640°C and the heat treatment time being 0.5 to 50 hours. Preferably, the heat treatment is a staged heat preservation treatment, including the following treatment process:
[0046] Heat treatment at 140°C for 0.5-1h;
[0047] Heat treatment at 157°C for 1-3 hours;
[0048] Heat treatment at 200℃ for 1-3h;
[0049] Heat treatment at 250℃ for 1-3h;
[0050] Heat treatment at 300℃ for 1-3h;
[0051] Heat treatment at 350℃ for 1-5h;
[0052] Heat treatment at 400℃ for 1-5h;
[0053] Heat treatment at 450℃ for 1-5h;
[0054] Heat treatment at 500℃ for 1-5h;
[0055] Heat treatment at 550℃ for 1-5h;
[0056] Heat treatment at 600℃ for 1-5h;
[0057] Heat treatment at 630℃ for 1-6h.
[0058] The heat treatment process of this embodiment of the present invention preferably adopts a segmented heat preservation treatment method, which can prevent the solder from melting and flowing out, while ensuring the uniformity of the solder. By gradually increasing the temperature, the solder indium and the like gradually form a high melting point alloy with aluminum.
[0059] S3. Cooling the rare earth rotary target after heat treatment to room temperature and cleaning it.
[0060] The rare earth rotating target prepared by the above method has a target welding rate of more than 95% and a solder melting point of more than 400°C. The sputtering power density of the target is more than 30% higher than that of pure indium welding, with a power density of 2-12W / cm 2 , preferably 6-10W / cm 2 ; The target material utilization rate is as high as over 88%.
[0061] Specific examples and experimental data are given below:
[0062] Example 1:
[0063] The total length of the rotating target is 1600mm, and it is made up of 9 terbium target tubes. The target tubes at both ends are dog-bone shaped, with outer diameters of 165mm and 158mm respectively, and the outer diameter of the middle area is 158mm. The gap between the target tube and the back tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of two 0.125mm thick aluminum rings. The aluminum content in the weld layer is 10%. The welding is completed at 220℃. The heat treatment process is as follows: 1) 140℃-0.5h; 2) 157℃ -1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h. The total heat treatment time is 35h. The melting point of the solder reaches 600℃ and the soldering rate is >95%. The sputtering target power is 5W / cm 2 , target utilization rate is 90%, aluminum content deviation is ±0.1%, and Tb content in the solder layer is <10ppm.
[0064] Example 2:
[0065] Sputtering target power is 8W / cm 2 , the other conditions are the same as in Example 1.
[0066] Example 3:
[0067] The sputtering target power is 10W / cm 2, the other conditions are the same as in Example 1.
[0068] Example 4:
[0069] It consists of one 0.05 mm and two 0.1 mm aluminum sheets, and the other conditions are the same as those in Example 1.
[0070] Example 5:
[0071] The sputtering target power is 12W / cm 2 , the other conditions are the same as in Example 1.
[0072] Example 6: The target material is dysprosium, and the rest is the same as Example 6.
[0073] Example 7: The target material is gadolinium and consists of two 0.125 mm aluminum sheets with an aluminum content of 10%. Other conditions are the same as those in Example 1.
[0074] Example 8: The target material is yttrium, consisting of one 0.05 mm piece and two 0.1 mm aluminum pieces. The other conditions are the same as those in Example 1.
[0075] Example 9:
[0076] The rotating target is 1500mm long and is made of six scandium target tubes. The target tubes at both ends are dog-bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the backing tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.05mm and one 0.08mm thick aluminum ring. The aluminum content in the weld layer is 5%, and welding is completed at 210℃. Heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0077] Example 10:
[0078] The rotating target is 1500mm long and is made of six ytterbium target tubes. The target tubes at both ends are dog-bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the backing tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.06mm and one 0.1mm thick aluminum ring. The aluminum content in the weld layer is 6%, and the welding is completed at 210℃. Heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0079] Example 11:
[0080] The total length of the rotating target is 1500mm, and it is made up of 6 lanthanum target tubes. The target tubes at both ends are dog bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the back tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.05mm, one 0.06mm and one 0.1mm thick aluminum ring. The aluminum content in the welding layer is 8%. It is completed at 210℃. Welding; heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0081] Example 12:
[0082] The rotating target is 1500mm long and is made up of six holmium target tubes. The target tubes at both ends are dog-bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the backing tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.05mm and two 0.1mm thick aluminum rings. The aluminum content in the weld layer is 10%. Welding is completed at 210℃. Heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0083] Example 13:
[0084] The total length of the rotating target is 1500mm, and it is made up of 7 sections of erbium target tubes. The target tubes at both ends are dog bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the back tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.07mm, one 0.08mm, and one 0.1mm thick aluminum ring. The aluminum content in the weld layer is 10%. At 210℃ Complete welding; heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0085] Example 14:
[0086] The rotating target is 1500mm long and is made of eight samarium target tubes. The target tubes at both ends are dog-bone shaped, with outer diameters of 112mm and 108mm respectively, and the outer diameter of the middle area is 108mm. The gap between the target tube and the backing tube is 1mm. The aluminum sheet is cylindrical and concentric with the target tube. It consists of one 0.1mm and one 0.15mm thick aluminum ring. The aluminum content in the weld layer is 10%. Welding is completed at 210℃. Heat treatment process: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 500℃-3h; 10) 550℃-4h; 11) 600℃-4h; 12) 630℃-4h.
[0087] Comparative Example 1:
[0088] The total length of the rotating target is 1600mm, and it is made up of 9 terbium target tubes. The outer diameters of A4 and A1 at the dog head are 165mm and 158mm respectively, and the outer diameter of the middle area is 158mm. The gap between the target tube and the back tube is 1mm. There is no aluminum sheet, and the aluminum content in the weld layer is 0%. Welding is completed at 220℃, and the welding rate is >95%. The sputtering target power is 5W / cm 2 , target utilization rate is 82%.
[0089] Comparative Example 2: Sputtering target power is 6W / cm 2 , the other conditions are the same as those in comparative example 1, and the target material is desoldered during the coating process.
[0090] Comparative Example 3: It is composed of 2 0.02 mm, 2 0.03 mm and 1 0.15 mm aluminum sheets, and the other conditions are the same as those in Example 1.
[0091] Comparative Example 4: It consists of one 0.25 mm aluminum sheet, and the other conditions are the same as those of Example 1.
[0092] Comparative Example 5:
[0093] The target material structure is the same as that in Example 1, but the heat treatment process is different. The heat treatment process is: 1) 140℃-0.5h; 2) 157℃-3h; 3) 200℃-4h; 4) 300℃-5h; 5) 400℃-10h; 6) 500℃-10h; 7) 630℃-17.5h, and the total heat treatment time is 50h.
[0094] Comparative Example 6: The heat treatment process was 630°C for 17.5h, and the other conditions were the same as those in Example 1.
[0095] Comparative Example 7:
[0096] The target material structure is the same as that in Example 1, consisting of a piece of aluminum sheet with a thickness of 0.13 mm, the aluminum content in the welding layer is 5%, and the heat treatment process is: 1) 140℃-0.5h; 2) 157℃-1.5h; 3) 200℃-1.5h; 4) 250℃-1.5h; 5) 300℃-2h; 6) 350℃-3h; 7) 400℃-3h; 8) 450℃-3h; 9) 480℃-3h.
[0097] Comparative Example 8: Consists of 1 piece of 0.05mm aluminum sheet with an aluminum content of 2%. The heat treatment time is 1) 140℃-0.5h; 2) 157℃-3h; 3) 200℃-4h; 4) 300℃-5h; 5) 330℃-10h. The other conditions are the same as those in Example 1.
[0098] Comparative Example 9: Consists of one 0.07 mm, one 0.1 mm, and two 0.15 mm aluminum sheets, with an aluminum content of 15%. Other conditions are the same as those in Example 1.
[0099] Comparative Example 10: The total length of the rotating target is 1600 mm. It is composed of 9 terbium target tubes. The target tubes at both ends are dog-bone shaped with outer diameters of 165 mm and 158 mm respectively. The outer diameter of the middle area is 158 mm. The gap between the target tube and the back tube is 1 mm. The aluminum sheet is columnar and concentric with the target tube. Solder with an aluminum content of 10% is used for welding. The welding is completed at 650°C, and the sputtering target power is 5 W / cm2.
[0100] Tables 1 and 2 show the performance parameter comparisons of the above embodiments and comparative examples.
[0101] Table 1 Performance parameters of various embodiments and comparative examples (1)
[0102]
[0103]
[0104]
[0105] Table 2 Performance parameters of various embodiments and comparative examples (2)
[0106]
[0107] As can be seen from Tables 1 and 2 above, the rare earth rotary target material and the preparation method thereof provided by the technical solution of the embodiment of the present invention can improve the sputtering target power and target utilization rate by adding aluminum sheets during the low-temperature welding process and combining the heat treatment process:
[0108] (1) Compared with pure indium welding, adding aluminum sheets (aluminum content 3-10%) to the welding layer can improve the target utilization rate, and the target utilization rate is increased from 82% to more than 89%.
[0109] (2) Compared with pure indium welding, adding aluminum sheets to the welding layer can significantly increase the melting point of the solder. The melting point is increased to above 400 ° C, which is beneficial to increase the power of the sputtering target and ensure that the target is not desoldered, that is, the solder is not melted, and the back tube and the target tube do not slide. The target power is increased from 5W / cm 2 Increased to 6-12W / cm 2 .
[0110] (3) A reasonable heat treatment process can shorten the total heat treatment time, make the solder melting point close to the theoretical melting point, and reduce the contamination of the solder on the target material, preventing open welding in the later stage. It also overcomes the problem that the one-step heating process will cause the solder to melt, contaminate the target material, and cause the target material component in the solder layer to be too high.
[0111] (4) The thickness of a single aluminum sheet is controlled within 0.05-0.15mm, which is beneficial to improving the utilization rate of the target material, increasing the sputtering power density, and reducing the contamination of the target material by the solder layer. If the thickness of a single aluminum sheet is too thick, it will make it difficult to control the melting point of the solder. In this case, you can choose to combine multiple aluminum sheets to achieve better control of the solder melting point.
[0112] (5) Compared with the conventional indium welding temperature of 220°C, if 600°C solder is used, the welding temperature needs to exceed 600°C. However, the embodiment provided by the present invention can achieve welding at 220°C. The melting point of the solder can be increased to 600°C through treatment, which reduces the welding difficulty, reduces the contamination of the solder to the target material, and improves the target sputtering power density.
[0113] In summary, embodiments of the present invention relate to a rare earth rotating target and its preparation method, suitable for use as a rare earth metal and alloy target for magnetic material coating, grain boundary diffusion, storage, and electronic information applications. The rare earth rotating target comprises a back tube and at least one rare earth target tube welded to the exterior of the back tube. The back tube and rare earth target tube are welded together via an intermediate weld layer comprising metallic indium solder and at least one aluminum sheet disposed within the indium solder, wherein the aluminum content of the intermediate weld layer is 3-10 wt.%. The back tube, aluminum sheet, and rare earth target tube form concentric cylindrical structures. The technical solution of the embodiments of the present invention addresses target welding and solder alloying. By adding an aluminum sheet within the weld layer and combining it with a heat treatment process, the solder melting point is increased from 156.6°C to above 400°C, significantly improving the sputtering target power density, thereby increasing the sputtering power density and target utilization of the rare earth rotating target, achieving low-temperature welding and slowing down rare earth target oxidation.
[0114] It should be understood that the above-described specific embodiments of the present invention are merely illustrative or illustrative of the principles of the present invention and do not constitute limitations of the present invention. Therefore, any modifications, equivalent substitutions, improvements, etc. made without departing from the spirit and scope of the present invention should be included within the scope of protection of the present invention. In addition, the appended claims are intended to cover all variations and modifications that fall within the scope and metes and bounds of the appended claims, or equivalents thereof.
Claims
1. A method for preparing a rare earth rotary target, characterized in that: The rare earth rotary target material comprises a backing tube and at least one rare earth target tube welded to the outside of the backing tube; The back tube and the rare earth target tube are welded via an intermediate welding layer, wherein the intermediate welding layer comprises a metal indium solder and at least one aluminum sheet disposed in the metal indium solder, wherein the aluminum content in the intermediate welding layer is 3-10 wt.%, and the back tube, the aluminum sheet, and the rare earth target tube are concentric cylindrical structures. The preparation method comprises the following steps: At a preset welding temperature, a metal indium solder is filled between the back tube and the rare earth target tube, and an aluminum sheet is placed in the metal indium solder; or an aluminum sheet is placed in the metal indium solder in advance, and then the metal indium solder with the aluminum sheet is filled between the back tube and the rare earth target tube, and the back tube and the rare earth target tube are welded to obtain a welded rare earth rotating target material; The welded rare earth rotary target is subjected to heat treatment at a temperature of 140° C. to 640° C. for a time of 0.5 to 50 hours. The heat treatment is a segmented heat preservation treatment, including: Heat treatment at 140°C for 0.5-1h; Heat treatment at 157°C for 1-3 hours; Heat treatment at 200℃ for 1-3h; Heat treatment at 250℃ for 1-3h; Heat treatment at 300℃ for 1-3h; Heat treatment at 350℃ for 1-5h; Heat treatment at 400℃ for 1-5h; Heat treatment at 450℃ for 1-5h; Heat treatment at 500℃ for 1-5h; Heat treatment at 550℃ for 1-5h; Heat treatment at 600℃ for 1-5h; Heat treatment at 630℃ for 1-6h; The rare earth rotary target after heat treatment is cooled to room temperature and cleaned.
2. The preparation method according to claim 1, characterized in that The rare earth target tube includes any one of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium and scandium.
3. The preparation method according to claim 1, characterized in that The thickness of a single aluminum sheet is 0.05-0.15 mm.
4. The preparation method according to any one of claims 1 to 3, characterized in that Also includes: Prior to filling, the aluminum sheet is pre-coated with a layer of metallic indium solder.
5. The preparation method according to any one of claims 1 to 3, characterized in that The preset welding temperature is 190-230°C.
6. The preparation method according to any one of claims 1 to 3, characterized in that The heat treatment comprises the following steps: Cooling the welded rare earth rotary target to room temperature and then cleaning it; The cleaned rare earth rotary target is placed in a vacuum heat treatment furnace and the vacuum is pumped to 10 -3 Below Pa; The rare earth rotary target is directly heat-treated or heat-treated after being filled with inert gas.
Citation Information
Patent Citations
Tubular target comprising a connecting layer that is situated between the tubular target and the tubular support
CN101080508A
Preparation method of high-purity rare earth and alloy target material
CN114231917A