Titanium-niobium alloy tube target material and preparation method thereof
By mixing titanium-niobium alloy powder and performing stepped hot isostatic pressing, the problems of cumbersome steps and low utilization rate in the preparation of titanium-niobium alloy tube targets were solved, and titanium-niobium alloy tube targets with high density and uniform structure were achieved, thereby improving the yield and sputtering performance.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-25
- Publication Date
- 2026-04-07
AI Technical Summary
Existing technologies for preparing titanium-niobium alloy tube targets suffer from cumbersome procedures, low utilization rates, and uneven composition. In particular, the melt casting method is prone to causing Nb infusible blocks, the spraying method results in high oxygen content, and the extrusion method produces poor microstructure uniformity.
Titanium-niobium alloy tube targets are prepared by mixing titanium metal powder and niobium metal powder in a predetermined mass ratio, followed by heat treatment and hot isostatic pressing with stepped heating through a cladding mold, and then machining.
This simplified the process flow, improved the density and microstructure uniformity of the titanium-niobium alloy tube sputtering target, increased the yield, and met the performance requirements of sputtering targets.
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Figure CN121802371A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of refractory alloy powder metallurgy target preparation technology, specifically a titanium-niobium alloy tube target and its preparation method. Background Technology
[0002] Magnetron sputtering, as a type of PVD coating technology, has developed rapidly and gained widespread application due to its high speed, low temperature, fast coating speed, uniform coating, and stronger adhesion between the film and the workpiece. In recent years, decorative functional films have developed into a large industrial cluster, with a large number of decorative coated products entering the consumer market. Currently, the colors of the films that can be produced include golden yellow, green, coffee, bronze, gray, black, grayish black, and rainbow colors. The target materials used in the decorative coating field include Ti, Cr, Al, Nb, Zr, and W. Different colored films can be obtained by selecting the type, material, gas, and coating process parameters. Films prepared by co-sputtering with different targets can achieve better decorative effects. However, films obtained by co-sputtering with single-element targets have disadvantages such as uneven composition distribution and poor quality stability. TiNb alloy targets composed of Ti and Nb elements can produce a rich variety of interference colors through reactive sputtering (introducing nitrogen, oxygen, etc.) and precise control of process parameters. The TiNb alloy target sputtering process is simple to operate, stable, and produces uniform and consistent composition.
[0003] Target materials can be classified into planar targets and rotating targets according to their shape. Planar targets have a utilization rate of 20-30%, while rotating targets can achieve a utilization rate of 70-80%, and the coating uniformity is superior to that of planar targets. Currently, the main methods for preparing tubular targets include melt casting, spraying, extrusion, and hot isostatic pressing. Ti has a melting point of 1668℃ and a density of 4.5 g / cm³. 3 Nb has a melting point of 2468℃ and a density of 8.57 g / cm³. 3 The two have significant differences in melting point and density. The melt casting method can easily produce Nb infusible blocks, but the product has coarse grains and low tube target strength. The tube target obtained by the spraying method has a lower density and higher oxygen content. The product obtained by the extrusion method has poor uniformity of the structure of each part. The advantage of hot isostatic pressing technology is that it combines the advantages of hot pressing and isostatic pressing, with a low forming temperature, dense product, and excellent performance.
[0004] Patent application CN 102489951A discloses a method for preparing niobium tube targets for sputtering. This method first involves drilling holes in a niobium ingot with a diameter of 180-300 mm to remove the core, obtaining a niobium tube blank. The blank is then encased and sealed with a cladding material and heat-treated at 900-1100℃ for 1-2 hours. The heat-treated blank, now encased in cladding material, is then extruded at an extrusion ratio of 5-9 to obtain the niobium tube target. After straightening, the target is acid-washed, followed by vacuum heat treatment. Finally, machining is performed to remove the cladding material, yielding the niobium tube target. This method involves chemical reagents such as hydrofluoric acid and nitric acid, causing environmental pollution. Furthermore, the process involves numerous steps, including core removal, multiple vacuum heat treatments, and hot extrusion after melting and casting, resulting in low utilization. Summary of the Invention
[0005] The purpose of this invention is to provide a titanium-niobium alloy tube target and its preparation method in order to solve at least one of the above-mentioned technical problems.
[0006] In a first aspect, embodiments of the present invention provide a method for preparing a titanium-niobium alloy tube target, comprising: mixing titanium metal powder and niobium metal powder at a preset mass ratio to obtain a titanium-niobium mixed powder; loading the titanium-niobium mixed powder into a cladding mold, then welding the end cap of the cladding mold and pre-reserving a vent hole; performing heat treatment and vacuum degassing on the cladding mold, and then performing hot isostatic pressing treatment with stepped heating on the cladding mold to obtain a pressed cladding; machining the pressed cladding and removing the inner and outer cladding to obtain a titanium-niobium alloy tube target.
[0007] Optionally, the preset mass ratio of titanium metal powder to niobium metal powder is 1~60:40~99.
[0008] Optionally, the sleeve mold includes an outer sleeve and a back tube, the back tube being disposed inside the outer sleeve, and an upper end cap and a lower end cap being respectively disposed at both ends of the sleeve mold, the upper end cap being provided with an air guide hole, the air guide hole being connected to the air guide tube.
[0009] Optionally, the material of the back tube may include a titanium tube or a stainless steel tube with a surface coating.
[0010] Optionally, the purity of the titanium metal powder is not less than 99.9% and the particle size is not greater than 75 μm; the purity of the niobium metal powder is not less than 99.9% and the particle size is not greater than 90 μm.
[0011] Optionally, titanium metal powder and niobium metal powder are mixed at a preset mass ratio, including: placing titanium metal powder and niobium metal powder at a preset mass ratio into a three-dimensional mixer and mechanically ball-milling them uniformly under an argon atmosphere; wherein the ball-to-powder mass ratio is 3~2:1, the ball-milling time is 10~18h, and the balls are made of hard zirconium balls and / or zirconium oxide balls.
[0012] Optionally, the cladding mold is subjected to a stepped heating hot isostatic pressing treatment to obtain the pressed cladding, including: under an argon protective atmosphere, heating to a first preset temperature at a first preset heating rate for a first preset holding time and holding pressure of a first preset pressure; then heating to a second preset temperature at a second preset heating rate for a second holding time and holding pressure of a second preset pressure; continuing to heat to a third preset temperature at a third preset heating rate for a third holding time and holding pressure of a third preset pressure; after the holding and pressure holding are completed, cooling to a fourth preset temperature at a preset cooling rate for a fourth preset holding time; and finally cooling and depressurizing in the furnace to obtain the pressed cladding.
[0013] Optionally, the first preset heating rate includes 2~5℃ / min, the first preset temperature includes 200~300℃, the first preset time includes 1~2h, and the first preset pressure includes 30~60MPa; the second preset heating rate includes 3~5℃ / min, the second preset temperature includes 500~700℃, the second preset time includes 1~3h, and the second preset pressure includes 60~80MPa; the third preset heating rate includes 5~10℃ / min, the third preset temperature includes 800~1200℃, the third preset time includes 3~10h, and the third preset pressure includes 100~200MPa; the preset cooling rate includes 2~4℃ / min, the fourth preset temperature includes 400~500℃, and the fourth preset time includes 1~2h.
[0014] Secondly, embodiments of the present invention also provide a titanium-niobium alloy tube target material, which is prepared by the preparation method provided in embodiments of the present invention.
[0015] Optionally, the mass fraction ratio of titanium to niobium in the titanium-niobium alloy tube target is 1~60:40~99.
[0016] This invention provides a titanium-niobium alloy tube target and its preparation method. The preparation process is simple, short in cycle, and low in cost, enabling the preparation of large-size TiNb alloy tube targets. Furthermore, through step-heating hot isostatic pressing, the prepared TiNb alloy tube target exhibits uniform microstructure and isotropic structure, with a TiNb alloy powder bonding rate approaching 100%. This invention alleviates the technical problems of cumbersome steps and low utilization rate in existing technologies. Attached Figure Description
[0017] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of this application. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.
[0018] Figure 1 This is a flowchart illustrating a method for preparing a titanium-niobium alloy tube target, as provided in an embodiment of the present invention. Detailed Implementation
[0019] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0020] Figure 1 This is a flowchart illustrating a method for preparing a titanium-niobium alloy tube target according to an embodiment of the present invention. Figure 1 As shown, the method specifically includes the following steps: Step S102: Titanium metal powder and niobium metal powder are mixed at a preset mass ratio to obtain titanium-niobium mixed powder. Preferably, the preset mass ratio of titanium metal powder to niobium metal powder is 1~60:40~99.
[0021] Step S104: The titanium-niobium mixed powder is loaded into the cladding mold, and then the end cap of the cladding mold is welded and a vent hole is reserved.
[0022] Specifically, the encapsulation mold includes an outer sleeve and a back tube, with the back tube located inside the outer sleeve. The two ends of the encapsulation mold are respectively provided with an upper end cap and a lower end cap. An air guide hole is provided on the upper end cap, and the air guide hole is connected to the air guide tube.
[0023] Preferably, the material of the back tube includes a titanium tube or a stainless steel tube with a surface coating. The stainless steel tube is coated with copper, nickel, or titanium, and the coating thickness is 0.1-1.0 mm.
[0024] In this embodiment of the invention, the back tube is filled with supporting material to prevent the back tube from shrinking and deforming under high temperature and high pressure, which would cause the product to be scrapped.
[0025] Step S106: The shroud mold is subjected to heat treatment and vacuum degassing, and then the shroud mold is subjected to hot isostatic pressing treatment with stepped heating to obtain the pressed shroud.
[0026] Step S108: The pressed casing is machined and the inner and outer casings are removed to obtain the titanium-niobium alloy tube target.
[0027] Preferably, in this embodiment of the invention, the titanium metal powder has a purity of not less than 99.9% and a particle size of not more than 75 μm. For example, the titanium metal powder has a purity of 99.9%, 99.95%, or 99.99% and a particle size of 70 μm, 60 μm, or 45 μm.
[0028] The purity of niobium metal powder is not less than 99.9%, and the particle size is not greater than 90 μm. For example, the purity of niobium metal powder is one of 99.9%, 99.95%, and 99.99%, and the particle size is one of 90 μm, 80 μm, and 60 μm.
[0029] Specifically, step S102 further includes the following steps: placing titanium metal powder and niobium metal powder of a preset mass ratio into a three-dimensional mixer and mechanically ball-milling them uniformly under argon atmosphere protection.
[0030] The ball-to-powder mass ratio is 3~2:1, the ball milling time is 10~18h, and the ball material is hard zirconium balls and / or zirconium oxide balls.
[0031] Preferably, in step S106, during the heat treatment and vacuum degassing of the casing mold, the heat treatment temperature is 400~800℃ and the holding time is 6~12h; after vacuum heat degassing, the vacuum degree inside the casing should be ≤10E-4Pa.
[0032] Specifically, step S106 involves performing a stepped heating hot isostatic pressing treatment on the shroud mold to obtain the pressed shroud, which includes the following steps: Step S1061: Under an argon protective atmosphere, the temperature is raised to a first preset temperature at a first preset heating rate for the first heat preservation, the heat preservation time is a first preset time, and the heat preservation pressure is a first preset pressure. The first preset heating rate includes 2~5℃ / min, the first preset temperature includes 200~300℃, the first preset time includes 1~2h, and the first preset pressure includes 30~60MPa. Step S1062, then heat up to the second preset temperature at the second preset heating rate and perform a second heat preservation, the heat preservation time is the second preset time, and the heat preservation pressure is the second preset pressure; The second preset heating rate includes 3~5℃ / min, the second preset temperature includes 500~700℃, the second preset time includes 1~3h, and the second preset pressure includes 60~80MPa. Step S1063: Continue heating at the third preset heating rate to the third preset temperature for a third heat preservation, the heat preservation time is the third preset time, and the heat preservation pressure is the third preset pressure; Among them, the third preset heating rate includes 5~10℃ / min, the third preset temperature includes 800~1200℃, the third preset time includes 3~10h, and the third preset pressure includes 100~200MPa; Step S1064: After the heat preservation and pressure preservation are completed, the temperature is cooled down to the fourth preset temperature at a preset cooling rate, and the heat preservation time is the fourth preset time. Among them, the preset cooling rate includes 2~4℃ / min, the fourth preset temperature includes 400~500℃, and the fourth preset time includes 1~2h; In step S1065, the furnace is finally cooled and depressurized to obtain the compressed casing.
[0033] The present invention also provides a titanium-niobium alloy tube target, which is prepared by the method provided in the embodiments of the present invention. The mass fraction ratio of titanium to niobium in the titanium-niobium alloy tube target is 1~60:40~99.
[0034] Example 1 A method for producing a TiNb alloy target, wherein the TiNb alloy composition is: Ti 42wt%, Nb 58wt%. The steps are as follows: According to the above target material composition design requirements, weigh Ti powder and Nb powder with a purity of 99.95%. Mix them in an argon atmosphere at a ball-to-powder mass ratio of 3:1 using a three-dimensional mixer for 10 hours to obtain a mixed powder. Prepare a carbon steel sheath, a 304 stainless steel back tube, and supporting materials. The outer surface of the 304 stainless steel back tube is plated with a Cu layer. Load the mixed powder into an annular cavity formed by the inner surface of the sheath and the outer surface of the back tube. Weld the upper and lower end caps to seal, leaving a degassing hole connected to a degassing pipe. Place the sheath in a heat treatment furnace for heat treatment and vacuum degassing. Hold at 600℃ for 6 hours. After the holding time, the vacuum degree inside the sheath should be ≤10E-4Pa.
[0035] The heat-treated cladding is then subjected to hot isostatic pressing (HIP). The HIP process is as follows: First, under an argon protective atmosphere, the temperature is increased to 200℃ at a rate of 2℃ / min for the first holding, and held for 2 hours, with the pressure controlled at 50MPa. Then, the temperature is increased to 500℃ at a rate of 5℃ / min for the second holding, and held for 3 hours, with the pressure controlled at 80MPa. Next, the temperature is increased to 800℃ at a rate of 10℃ / min for the third holding, and held for 8 hours, with the pressure controlled at 200MPa. After the holding and pressure maintenance, the temperature is decreased to 400℃ at a rate of 4℃ / min and held for 2 hours. Then, the temperature and pressure are continuously reduced along with the furnace.
[0036] After machining, a Ti42Nb 58wt% alloy tube sputtering material was obtained. The density of the Ti42Nb 58wt% alloy tube sputtering material is ≥99%, and the actual test result is 99.3%.
[0037] Example 2 A method for producing a TiNb alloy target, wherein the TiNb alloy composition is: Ti 50wt%, Nb 50wt%. The steps are as follows: According to the above target material composition design requirements, weigh Ti powder and Nb powder with a purity of 99.95%. Mix them in an argon atmosphere at a ball-to-powder mass ratio of 2:1 using a three-dimensional mixer for 12 hours to obtain a mixed powder. Prepare a carbon steel sheath, a 304 stainless steel back tube, and supporting materials. The outer surface of the 304 stainless steel back tube is plated with a Ti layer. Fill the mixed powder into an annular cavity formed by the inner surface of the sheath and the outer surface of the back tube. Weld the upper and lower end caps to seal them, leaving a degassing hole connected to a degassing pipe. Place the sheath in a heat treatment furnace for heat treatment and vacuum degassing. Hold at 800℃ for 10 hours. After the holding time, the vacuum degree inside the sheath should be ≤10E-4Pa.
[0038] The heat-treated cladding is then subjected to hot isostatic pressing (HIP). The HIP process is as follows: First, under an argon protective atmosphere, the temperature is increased to 300℃ at a rate of 2℃ / min for the first holding, and held for 1.5 hours, with the pressure controlled at 40MPa. Then, the temperature is increased to 600℃ at a rate of 4℃ / min for the second holding, and held for 2 hours, with the pressure controlled at 80MPa. Next, the temperature is increased to 1100℃ at a rate of 6℃ / min for the third holding, and held for 6 hours, with the pressure controlled at 150MPa. After the holding and pressure maintenance, the temperature is decreased to 500℃ at a rate of 2℃ / min and held for 2 hours. Then, the temperature and pressure are continuously reduced along with the furnace.
[0039] After machining, a Ti50Nb 50wt% alloy sputtering target is obtained. The density of the Ti50Nb 50wt% alloy tube sputtering target is ≥99%, and the actual test result is 99.8%.
[0040] Example 3 A method for producing a TiNb alloy target, wherein the TiNb alloy composition is: Ti 5wt%, Nb 95wt%. The steps are as follows: According to the above target material composition design requirements, weigh Ti powder and Nb powder with a purity of 99.95%. Mix them in an argon atmosphere at a ball-to-powder mass ratio of 3:1 using a three-dimensional mixer for 10 hours to obtain a mixed powder. Prepare a carbon steel sheath, a 304 stainless steel back tube, and supporting materials. The outer surface of the 304 stainless steel back tube is plated with a Cu layer. Load the mixed powder into an annular cavity formed by the inner surface of the sheath and the outer surface of the back tube. Weld the upper and lower end caps to seal, leaving a degassing hole connected to a degassing pipe. Place the sheath in a heat treatment furnace for heat treatment and vacuum degassing. Hold at 600℃ for 6 hours. After the holding time, the vacuum degree inside the sheath should be ≤10E-4Pa.
[0041] The heat-treated cladding is then subjected to hot isostatic pressing (HIP). The HIP process is as follows: First, under an argon protective atmosphere, the temperature is increased to 200℃ at a rate of 2℃ / min for the first holding, and held for 2 hours, with the pressure controlled at 50MPa. Then, the temperature is increased to 500℃ at a rate of 5℃ / min for the second holding, and held for 3 hours, with the pressure controlled at 80MPa. Next, the temperature is increased to 870℃ at a rate of 10℃ / min for the third holding, and held for 8 hours, with the pressure controlled at 200MPa. After the holding and pressure maintenance, the temperature is decreased to 400℃ at a rate of 4℃ / min and held for 2 hours. Then, the temperature and pressure are continuously reduced along with the furnace.
[0042] After machining, a Ti5Nb 95wt% alloy sputtering target was obtained. The density of the Ti5Nb 95wt% alloy tube sputtering target is ≥99%, and the actual test result is 99.1%.
[0043] Example 4 A method for producing a TiNb alloy tube target is disclosed. The production process steps of the TiNb alloy tube target differ from those in Example 3 in that the TiNb alloy composition is: Ti 60wt%, Nb 40wt%. The final Ti60Nb40wt% alloy tube target material has a density ≥99%, and the actual test result is 99.4%.
[0044] Comparative Example 1 A method for producing a TiNb alloy tube target differs from that in Example 3 in that the hot isostatic pressing process is as follows: under an argon protective atmosphere, the temperature is increased to 870°C at a rate of 5°C / min, while the pressure is controlled at 200 MPa. Once both temperature and pressure reach the set values, the holding time is calculated and is 8 hours. After the holding time is completed, the furnace is cooled and the pressure is reduced. The density of the alloy target material obtained after machining is 97.2%.
[0045] Comparative Example 2 A method for producing a TiNb alloy tube target differs from that in Example 3 in that: firstly, under an argon protective atmosphere, the temperature is increased to 200℃ at a heating rate of 2℃ / min for a first holding time of 2 hours, with the pressure controlled at 50MPa; then, the temperature is increased to 500℃ at a heating rate of 5℃ / min for a second holding time of 3 hours, with the pressure controlled at 80MPa; next, the temperature is increased to 750℃ at a heating rate of 10℃ / min for a third holding time of 8 hours, with the pressure controlled at 200MPa; after the holding and pressure maintenance, the temperature is decreased to 400℃ at a cooling rate of 4℃ / min for a holding time of 2 hours; then, the temperature and pressure are continuously reduced in the furnace. After mechanical processing, a Ti5Nb 95wt% alloy target material is obtained. The density of the Ti5Nb 95wt% alloy tube target material is ≥99%, and the actual test result is 96.2%.
[0046] As can be seen from Examples 1-3 and Comparative Examples 1-2, the hot isostatic pressing treatment method with stepped heating provided in the embodiments of the present invention, as well as the temperature and pressure range provided in the embodiments of the present invention, can improve the density of titanium-niobium alloy tube targets.
[0047] As described above, this invention provides a titanium-niobium alloy tube target and its preparation method. The hot isostatic pressing integral molding process is key, which involves graded heating and pressurization, heat preservation and pressure holding, and cooling and depressurization treatment. This not only effectively improves the density and uniformity of the target material, but also avoids excessive grain growth, improves the yield of the tubular target, and meets the performance requirements of sputtering targets.
[0048] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or essential characteristics. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, all variations falling within the meaning and scope of equivalents of the claims are intended to be included within the present invention. No reference numerals in the claims should be construed as limiting the scope of the claims.
[0049] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A method for preparing a titanium-niobium alloy tube target, characterized in that, include: Titanium metal powder and niobium metal powder are mixed at a preset mass ratio to obtain titanium-niobium mixed powder; The titanium-niobium mixed powder is loaded into the encapsulation mold, and then the end cap of the encapsulation mold is welded and a vent hole is reserved. The encapsulation mold is subjected to heat treatment and vacuum degassing, and then subjected to hot isostatic pressing treatment with stepped heating to obtain the pressed encapsulation. The compressed casing is machined and the inner and outer casings are removed to obtain a titanium-niobium alloy tube target.
2. The method according to claim 1, characterized in that: The preset mass ratio of titanium metal powder to niobium metal powder is 1~60:40~99.
3. The method according to claim 1, characterized in that: The packaging mold includes an outer sleeve and a back tube. The back tube is disposed inside the outer sleeve. The two ends of the packaging mold are respectively provided with an upper end cap and a lower end cap. The upper end cap is provided with an air guide hole, which is connected to the air guide tube.
4. The method according to claim 3, characterized in that: The back tube is made of titanium or stainless steel with a surface coating.
5. The method according to claim 1, characterized in that: The purity of the titanium metal powder is not less than 99.9%, and the particle size is not greater than 75μm; The purity of the niobium metal powder is not less than 99.9%, and the particle size is not greater than 90 μm.
6. The method according to claim 1, characterized in that: Titanium metal powder and niobium metal powder are mixed at a preset mass ratio, including: Titanium metal powder and niobium metal powder with a preset mass ratio are placed into a three-dimensional mixer and mechanically ball-milled and mixed evenly under an argon atmosphere. The ball-to-powder mass ratio is 3~2:1, the ball milling time is 10~18h, and the ball material is hard zirconium balls and / or zirconium oxide balls.
7. The method according to claim 1, characterized in that: The encapsulation mold is subjected to hot isostatic pressing with stepped heating to obtain the pressed encapsulation, comprising: Under an argon protective atmosphere, the temperature is raised to a first preset temperature at a first preset heating rate for the first heat preservation, the heat preservation time is first preset time, and the heat preservation pressure is first preset pressure. Then, the temperature is raised to the second preset temperature at the second preset heating rate for a second heat preservation time and a second preset pressure. Continue heating at the third preset heating rate to the third preset temperature for a third heat preservation, with the heat preservation time being the third preset time and the heat preservation pressure being the third preset pressure. After the heat preservation and pressure holding are completed, the temperature is reduced to the fourth preset temperature at a preset cooling rate, and the heat preservation time is the fourth preset time. Finally, the furnace is cooled and depressurized to obtain the post-pressurization cladding.
8. The method according to claim 7, characterized in that: The first preset heating rate includes 2~5℃ / min, the first preset temperature includes 200~300℃, the first preset time includes 1~2h, and the first preset pressure includes 30~60MPa; The second preset heating rate includes 3~5℃ / min, the second preset temperature includes 500~700℃, the second preset time includes 1~3h, and the second preset pressure includes 60~80MPa; The third preset heating rate includes 5~10℃ / min, the third preset temperature includes 800~1200℃, the third preset time includes 3~10h, and the third preset pressure includes 100~200MPa; The preset cooling rate includes 2~4℃ / min, the fourth preset temperature includes 400~500℃, and the fourth preset time includes 1~2h.
9. A titanium-niobium alloy tube target, characterized in that, It is prepared by the method described in any one of claims 1-8.
10. The titanium-niobium alloy tube target according to claim 9, characterized in that: The mass fraction ratio of titanium to niobium in the titanium-niobium alloy tube target is 1~60:40~99.
Citation Information
Patent Citations
Preparation method of niobium tubular target materials for sputtering
CN102489951A