Molybdenum and / or molybdenum alloy tubular target material and preparation method thereof

Abstract

The invention provides a molybdenum and / or molybdenum alloy tubular target material and a preparation method thereof, and relates to the technical field of refractory metal target materials of flat panel display devices.The preparation method comprises the following steps that molybdenum powder and / or molybdenum alloy powder are / is subjected to cold isostatic pressing to obtain a tube blank, then the tube blank is subjected to shaping machining, and a pure molybdenum tubular pressed blank and / or a molybdenum alloy tubular pressed blank are / is obtained; assembling the tubular pressed blank single piece or multiple sections in a sheath, degassing and sealing the sheath, performing primary hot isostatic pressing, and removing the sheath through machining to obtain a pure molybdenum pipe and / or a molybdenum alloy pipe; and the at least two sections of pure molybdenum pipes and / or molybdenum alloy pipes are assembled in the large-size pipe sheath again, then secondary hot isostatic pressing is conducted on the large-size pipe sheath after degassing sealing is conducted on the large-size pipe sheath, and after the sheath is removed through machining, the molybdenum and / or molybdenum alloy tubular target material is obtained. The components of the target material can be flexibly adjusted according to design and requirements, and the molybdenum and / or molybdenum alloy tubular target material with high density and large size is obtained.

Description

Technical Field

[0001] This invention relates to the field of refractory metal target technology for flat panel display devices, and in particular to a molybdenum and / or molybdenum alloy tubular target and its preparation method. Background Technology

[0002] Molybdenum and molybdenum alloy sputtering targets are currently mainly used in the thin-film transistor liquid crystal display (TFT-LCD) and active-matrix organic light-emitting diode (AMOLED) panel display industries. Targets are fundamental consumables in the magnetron sputtering process, used in large quantities, and their quality plays a crucial role in determining the performance of the metal thin film. Tubular targets are more efficient and have a longer service life compared to planar targets. As display screens become larger and quality requirements increase, the required size and performance of molybdenum and molybdenum alloy targets also increase.

[0003] The main method for preparing large-size molybdenum and molybdenum alloy tube targets is powder metallurgy, which involves pressing the billet, sintering at high temperature, and then deforming it through extrusion / forging. Patent ZL2016109897187 discloses a method for manufacturing a molybdenum alloy rotating target, using molybdenum trioxide powder and hafnium to cast a tube blank, followed by cold isostatic pressing, sintering, extrusion, and machining. However, the presence of hafnium affects the purity of the molybdenum target, potentially impacting the performance of the subsequent sputtered thin film. Patent ZL2018103419528 discloses a method for preparing an integral tubular molybdenum target, using hollow forging of the sintered billet instead of extrusion, followed by forging, annealing, and machining. However, extensive deformation can lead to uneven grain structure and complex processes, affecting the quality consistency of large-size tube targets.

[0004] Hot isostatic pressing (HIP) is also a major method for preparing high-performance molybdenum and molybdenum alloy large-size tubular targets. Patent ZL2014108440669 discloses a method for preparing molybdenum alloy targets, using molybdenum powder and other alloying element powders for mechanical alloying, followed by cold isostatic pressing and then hot isostatic pressing. Tubular targets typically have larger dimensions at both ends than in the middle; direct hot isostatic pressing would increase the blank allowance, resulting in processing waste. Patent ZL2018110421861 provides a method for preparing tubular targets, including: cold isostatic pressing molybdenum powder into tubular blanks, followed by high-temperature sintering; then, longitudinally stacking multiple sintered tubular blanks within a casing, connecting and densifying them through hot isostatic pressing to form a long molybdenum tube target; finally, straightening the bent parts of the target and performing stress-relief annealing in a vacuum environment to obtain the finished product. However, this method has the following main drawbacks: First, its applicability is limited. Due to the use of a sintering-then-hot isostatic pressing route, the required temperature and pressure are high, making it particularly unsuitable for molybdenum alloys such as molybdenum-titanium and molybdenum-niobium, which cannot be sintered with hydrogen and can only be sintered in vacuum. These alloys have the problem of difficult-to-control sintering density. Second, the connection quality and machinability are poor. During hot isostatic pressing, the connection and fit between the segmented tube blanks are not high, and the whole is prone to deformation and cracking during straightening. Third, the process is cumbersome and difficult to control. To ensure that the gaps during stacking and splicing are as small as possible, each molybdenum tube blank needs to be repeatedly trimmed, which increases the complexity of preparation. At the same time, the annealing treatment after straightening can easily lead to coarse grains or new performance inhomogeneities in the bent parts, affecting the reliability of the final product.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The purpose of this invention is to provide a molybdenum and / or molybdenum alloy tubular target and its preparation method. By assembling multiple segments of molybdenum and / or molybdenum alloy tubular materials into a large-size tubular sheath and performing a secondary hot isostatic pressing treatment, a high-density, large-size, and compositionally adjustable molybdenum and / or molybdenum alloy tubular target is obtained. The method provided by this invention integrates significant advantages such as high flexibility, modular assembly, cost-effectiveness, strong adaptability to size and shape, and customizable composition, offering an efficient and reliable solution for the preparation of high-performance, large-size tubular targets.

[0007] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides a method for preparing a tubular target material of molybdenum and / or molybdenum alloy, comprising the following steps: S1: Provide molybdenum powder and / or molybdenum alloy powder; S2: Molybdenum powder and / or molybdenum alloy powder are cold isostatically pressed to obtain a tube blank, and then the tube blank is shaped to obtain a pure molybdenum tubular blank and / or a molybdenum alloy tubular blank. S3: Assemble one or more sections of pure molybdenum tubular blanks and / or molybdenum alloy tubular blanks in a cladding, and then degas and seal the cladding; S4: After the degassing and sealing of the casing, hot isostatic pressing is performed, and the casing is removed by machining to obtain pure molybdenum pipe and / or molybdenum alloy pipe; S5: Reassemble at least two sections of pure molybdenum pipe and / or molybdenum alloy pipe into a large-size pipe sheath, and then degas and seal the large-size pipe sheath. S6: After degassing and sealing, the large-size tubular casing is subjected to secondary hot isostatic pressing, and the casing is removed by machining to obtain a molybdenum and / or molybdenum alloy tubular target.

[0008] Furthermore, based on the above technical solution, the Fisher particle size of the molybdenum powder is 2.5~4.5μm; And / or, molybdenum alloy powder includes molybdenum powder and alloy powder; Alloy powders include one or more of titanium powder, nickel powder, and niobium powder; The particle size of both titanium powder and niobium powder is 325 mesh to -200 mesh; The Fisher particle size of nickel powder is 3~5μm; The purity of both molybdenum powder and alloy powder is greater than 99%.

[0009] Furthermore, based on the above technical solution, in step S1, the method for preparing the molybdenum alloy powder includes: mixing molybdenum powder and alloy powder using a dual-motion mixer, introducing a protective gas during the mixing process, with a gas pressure of 1.1-1.2 atmospheres, and a mixing time of 4-10 hours; The protective gas is argon, nitrogen, or helium.

[0010] Furthermore, based on the above technical solution, in step S2, molybdenum powder and / or molybdenum alloy powder are loaded into a tubular mold for cold isostatic pressing. The pressure of the cold isostatic pressing is 200-250 MPa, and the holding time is 5-15 min. And / or, in step S2, the shaping process refers to shaping through machining.

[0011] Furthermore, based on the above technical solution, in step S3, the degassing of the casing involves vacuuming the casing at a temperature of 500-600℃ for 6-10 hours until the gas pressure inside the casing is ≤10. -4 Pa.

[0012] Furthermore, based on the above technical solution, the conditions for the first hot isostatic pressing in step S4 include: Temperature: 850-1450℃; Pressure: 100-150MPa; Time: 1-6h; Specifically, when the molybdenum alloy pipe is a molybdenum-titanium alloy pipe, a molybdenum-titanium-nickel alloy pipe, or a molybdenum-nickel alloy pipe, the conditions for a single hot isostatic pressing include: a temperature of 900-1200℃, a pressure of 100-150MPa, and a time of 1-6h. When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for a single hot isostatic pressing include: temperature of 1200-1450℃, pressure of 100-150MPa, and time of 1-6h. When the pipe is pure molybdenum, the conditions for a single hot isostatic pressing include: temperature of 900-1200℃, pressure of 100-150MPa, and time of 1-6h. And / or, in step S4, the density of the obtained pure molybdenum tubing and / or molybdenum alloy tubing is ≥94.5%.

[0013] Furthermore, based on the above technical solution, in step S5, the large-size pipe sheath refers to assembling and splicing multiple sections of pure molybdenum pipe and / or multiple sections of molybdenum alloy pipe together, and then sheathing them. And / or, the length of the combined pipe in the large-size pipe sheath is 2.3 meters to 3.5 meters; And / or, degassing of large-size tube sheaths involves vacuum degassing of the large-size tube sheath at 500-600℃ for 6-10 hours until the gas pressure inside the sheath is ≤10. -4 Pa.

[0014] Furthermore, based on the above technical solution, the conditions for secondary hot isostatic pressing in step S6 include: Temperature: 950-1550℃; Pressure: 160-180MPa; Time: 3-10h; Specifically, when the molybdenum alloy pipe is a molybdenum-titanium alloy pipe, a molybdenum-titanium-nickel alloy pipe, or a molybdenum-nickel alloy pipe, the conditions for secondary hot isostatic pressing include: 950-1200℃, pressure of 160-180MPa, and time of 3-10h. When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for secondary hot isostatic pressing include: temperature of 1200-1550℃, pressure of 160-180MPa, and time of 3-10h. When the tubing is pure molybdenum, the conditions for secondary hot isostatic pressing include: 950-1200℃, pressure of 160-180MPa, and time of 3-10h. And / or, the temperature, pressure, and time of the secondary hot isostatic pressing are all greater than those of the primary hot isostatic pressing.

[0015] The present invention also provides a molybdenum and / or molybdenum alloy tubular target prepared by the method described above, which is composed of multiple pure molybdenum targets and / or multiple molybdenum alloy targets spliced ​​together.

[0016] Furthermore, based on the above technical solution, the molybdenum alloy target material includes one or more of the following: molybdenum-titanium alloy target material, molybdenum-titanium-nickel alloy target material, molybdenum-nickel alloy target material, molybdenum-titanium-niobium alloy target material, and molybdenum-niobium alloy target material. And / or, the length of the molybdenum and / or molybdenum alloy tubular target is 2.3 meters to 3.5 meters; And / or, the density of the molybdenum and / or molybdenum alloy tubular target is ≥99.5%; And / or, the oxygen content of the molybdenum and / or molybdenum alloy tubular target is 600-800 ppm.

[0017] The present invention provides a molybdenum and / or molybdenum alloy tubular target and its preparation method, the beneficial effects of which include at least the following: 1. The molybdenum and / or molybdenum alloy tubular target provided by the present invention has a large size and high density (≥99.5%). The composition of the target can be flexibly adjusted according to the design and requirements, thereby realizing the functionalization of specific areas of the overall target composition (optimizing the sputtering zone).

[0018] 2. The preparation method provided by the present invention, by assembling multiple sections of molybdenum and / or molybdenum alloy pipes into a large-size pipe sheath and performing secondary hot isostatic pressing treatment, can not only make the joints of the multiple pipe sections have high density, significantly improving the strength and structural integrity of the target material, but also make more effective use of raw materials and reduce the high scrap rate and huge processing costs caused by large integral forging or sintering. Attached Figure Description

[0019] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in 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 the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0020] Figure 1 This is a schematic diagram of the molybdenum-titanium alloy tubular target structure prepared in Example 1 of the present invention; Figure 2 This is a schematic diagram of the molybdenum and molybdenum-titanium alloy tubular target structure prepared in Example 4 of the present invention; Figure 3 The image shows the microstructure of the joint between two connected tubular sections in the molybdenum-titanium alloy tubular target prepared in Comparative Example 3. Detailed Implementation

[0021] To make the objectives, technical solutions, and advantages of this invention clearer, the technical solutions in the embodiments of this invention will be clearly and completely described below in conjunction with the embodiments of this invention. Those skilled in the art should understand that the embodiments described are merely illustrative of the invention and should not be considered as specific limitations thereof. All other embodiments obtained by those skilled in the art based on the embodiments of this invention without creative effort are within the scope of protection of this invention. Process parameters not specifically specified in the following embodiments are generally performed under conventional conditions.

[0022] The endpoints and any values ​​of the ranges disclosed in this invention are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoint values ​​of the various ranges, the endpoint values ​​of the various ranges and individual point values, and individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered as specifically disclosed in this invention.

[0023] According to a first aspect of the present invention, a method for preparing a molybdenum and / or molybdenum alloy tubular target is provided, comprising the following steps: S1: Provide molybdenum powder and / or molybdenum alloy powder; S2: Molybdenum powder and / or molybdenum alloy powder are cold isostatically pressed to obtain a tube blank, and then the tube blank is shaped to obtain a pure molybdenum tubular blank and / or a molybdenum alloy tubular blank. S3: Assemble one or more sections of pure molybdenum tubular blanks and / or molybdenum alloy tubular blanks in a cladding, and then degas and seal the cladding; S4: After the degassing and sealing of the casing, hot isostatic pressing is performed, and the casing is removed by machining to obtain pure molybdenum pipe and / or molybdenum alloy pipe; S5: Reassemble at least two sections of pure molybdenum pipe and / or molybdenum alloy pipe into a large-size pipe sheath, and then degas and seal the large-size pipe sheath. S6: After degassing and sealing, the large-size tubular casing is subjected to secondary hot isostatic pressing, and the casing is removed by machining to obtain a molybdenum and / or molybdenum alloy tubular target.

[0024] Specifically, this invention uses secondary hot isostatic pressing to allow sufficient atomic diffusion at the interface of segmented pipes, forming a strong metallurgical bond. This solves the problems of defects, inclusions, or weak bonding areas that may result from traditional welding or mechanical connections. As a result, the assembled pipe target is equivalent to a one-time formed whole in terms of microstructure and mechanical properties. This not only gives the target material a high density but also enables more effective use of raw materials, reducing the high scrap rate and huge processing costs associated with large-scale integral forging or sintering.

[0025] As an optional embodiment of the present invention, the molybdenum powder has a Fisher particle size of 2.5~4.5μm (e.g., 3μm, 3.5μm, 4μm, etc.). Molybdenum alloy powder includes molybdenum powder and alloy powder; Alloy powders include one or more of titanium powder, nickel powder, and niobium powder; The particle size of both titanium powder and niobium powder is 325 mesh to -200 mesh; The Fisher particle size of nickel powder is 3~5μm (e.g., 3.5μm, 4μm, 4.5μm, etc.). The purity of both molybdenum powder and alloy powder is greater than 99%.

[0026] As an optional embodiment of the present invention, in step S1, the method for preparing molybdenum alloy powder includes: mixing molybdenum powder and alloy powder using a dual-motion mixer, introducing a protective gas during the mixing process to remove air and reduce oxygen content, with a gas pressure of 1.1-1.2 atmospheres and a mixing time of 4-10 hours (e.g., 5 hours, 7 hours, 9 hours, etc.). The protective gas is argon, nitrogen, or helium.

[0027] As an optional embodiment of the present invention, in step S2, molybdenum powder and / or molybdenum alloy powder are loaded into a tubular mold for cold isostatic pressing. The pressure of the cold isostatic pressing is 200-250 MPa (e.g., 210 MPa, 220 MPa, 230 MPa, 240 MPa, etc.), and the holding time is 5-15 min (e.g., 7 min, 9 min, 10 min, 13 min, 14 min, etc.).

[0028] As an optional embodiment of the present invention, in step S2, the shaping process refers to shaping through machining.

[0029] In an optional embodiment of the present invention, in step S3, the degassing of the casing involves subjecting the casing to a long-term vacuum degassing process at a temperature of 500-600°C for 6-10 hours until the gas pressure inside the casing is ≤10. -4 Pa.

[0030] As an optional embodiment of the present invention, in step S4, the first hot isostatic pressing is performed in a HIP equipment; if the length of a single tube blank is ≤1 meter, most conventional HIP equipment can be used to reduce HIP costs. In step S4, the conditions for primary hot isostatic pressing include: Temperature ranges from 850 to 1450℃ (e.g., 900℃, 950℃, 1000℃, 1100℃, 1200℃, 1300℃, 1350℃, 1400℃, etc.), pressure ranges from 100 to 150 MPa (e.g., 100 MPa, 120 MPa, 140 MPa, etc.), and time ranges from 1 to 6 hours (e.g., 2 hours, 3 hours, 4 hours, 5 hours, etc.). When the molybdenum alloy pipe is a molybdenum-titanium or molybdenum-titanium-nickel alloy or molybdenum-nickel alloy pipe, the conditions for a single hot isostatic pressing include: a temperature of 900-1200℃ (e.g., 900℃, 950℃, 1000℃, 1100℃, 1150℃, etc.), a pressure of 100-150MPa (e.g., 110MPa, 120MPa, 140MPa, 145MPa, etc.), and a time of 1-6h (e.g., 2h, 3h, 4h, 5h, etc.). When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for a single hot isostatic pressing include: a temperature of 1200-1450℃ (e.g., 1250℃, 1300℃, 1350℃, 1400℃, etc.), a pressure of 100-150MPa (e.g., 110MPa, 120MPa, 140MPa, 145MPa, etc.), and a time of 1-6h (e.g., 2h, 3h, 4h, 5h, etc.). When using pure molybdenum tubing, the conditions for a single hot isostatic pressing (HIP) process include: a temperature of 900-1200℃ (e.g., 900℃, 950℃, 1000℃, 1100℃, 1150℃, etc.), a pressure of 100-150MPa (e.g., 110MPa, 120MPa, 140MPa, 145MPa, etc.), and a time of 1-6h (e.g., 2h, 3h, 4h, 5h, etc.). In step S4, the density of the obtained pure molybdenum tubing and / or molybdenum alloy tubing is ≥94.5%.

[0031] Specifically, if the temperature of the first hot isostatic pressing is too high, it will lead to abnormally coarse grains, significantly reducing the strength and toughness of the material. For alloys such as molybdenum-titanium and molybdenum-niobium, it may also cause segregation or inhomogeneity of alloy element composition. Conversely, if the temperature of the first hot isostatic pressing is too low, the atomic diffusion rate will be too slow, and it will be impossible to effectively achieve pore closure and sufficient growth of sintering necks. As a result, the billet has low density and a large number of closed pores. Performing a second HIP on the billet with low density will force the second HIP to undertake a heavier densification task, which may damage the bonding quality or require more extreme parameters, increasing the overall process risk.

[0032] Furthermore, if the pressure of the first hot isostatic pressing is too high, the billet size will deviate significantly from the design, and the original small defects or areas of uneven density inside the billet may expand into microcracks due to the huge pressure; conversely, if the pressure of the first hot isostatic pressing is too low, the material cannot produce enough creep at high temperature to fill the internal pores, leaving open pores and network pores in the billet, which prevents the density from being increased.

[0033] As an optional embodiment of the present invention, the large-size pipe sheath refers to assembling and splicing multiple sections of pure molybdenum pipe and / or multiple sections of molybdenum alloy pipe together, and then sheathing them.

[0034] As an optional embodiment of the present invention, in step S5, the degassing of the large-size tube sheath involves subjecting the large-size tube sheath to a long-term vacuum degassing process at a temperature of 500-600℃ (e.g., 520℃, 540℃, 560℃, 580℃, etc.) for 6-10 hours (e.g., 6 hours, 8 hours, 9 hours, etc.) until the gas pressure inside the sheath is ≤10. -4 Pa.

[0035] As an optional embodiment of the present invention, in step S6, the secondary hot isostatic pressing is performed in a large-size (e.g., 2.3 m to 3.5 m long) HIP device; the length of the combined pipe in the large-size pipe sheath is 2.3 m to 3.5 m; In step S6, the conditions for secondary hot isostatic pressing include: The temperature is 950-1550℃ (e.g., 1000℃, 1300℃, 1400℃, 1500℃, etc.), the pressure is 160-180MPa (e.g., 165MPa, 170MPa, 175MPa, etc.), and the time is 3-10h (e.g., 5h, 7h, 9h, etc.). When the molybdenum alloy pipe is a molybdenum-titanium alloy pipe, a molybdenum-titanium-nickel alloy pipe, or a molybdenum-nickel alloy pipe, the conditions for secondary hot isostatic pressing include: a temperature of 950-1200℃ (e.g., 1000℃, 1050℃, 1100℃, 1150℃, etc.), a pressure of 160-180MPa (e.g., 165MPa, 170MPa, 175MPa, etc.), and a time of 3-10h (e.g., 5h, 7h, 9h, etc.). When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for secondary hot isostatic pressing include: temperature of 1200-1550℃ (e.g., 1250℃, 1300℃, 1400℃, 1500℃, etc.), pressure of 160-180MPa (e.g., 165MPa, 170MPa, 175MPa, etc.), and time of 3-10h (e.g., 5h, 7h, 9h, etc.). When the tubing is pure molybdenum, the conditions for secondary hot isostatic pressing include: 950-1200℃ (e.g., 950℃, 1000℃, 1100℃, 1150℃, etc.), pressure of 160-180MPa (e.g., 165MPa, 170MPa, 175MPa, etc.), and time of 3-10h (e.g., 5h, 7h, 9h, etc.). The temperature, pressure, and time of the secondary hot isostatic pressing are all greater than those of the primary hot isostatic pressing.

[0036] Specifically, this invention limits the temperature, pressure, and time of secondary hot isostatic pressing to be greater than those of primary hot isostatic pressing because primary HIP mainly achieves pore closure and densification within a single material, with a relatively direct driving force. In contrast, secondary HIP mainly achieves atomic-level diffusion and metallurgical bonding between different material segments (such as pure molybdenum and molybdenum alloys) or between segments of the same material. Microscopic unevenness, oxide films, or contamination layers usually exist at the interface, which can hinder atomic bonding. Therefore, secondary HIP needs to provide a higher thermodynamic driving force (higher temperature provides stronger atomic diffusion capability, and higher pressure promotes microscopic plastic rheology to destroy the barrier layer) and a longer kinetic process (longer time to ensure sufficient diffusion) in order to achieve a perfect bond with properties indistinguishable from the parent material.

[0037] Furthermore, if the temperature of the secondary hot isostatic pressing is too high, it will cause local grain coarsening or softening of the target tube, which will easily lead to distortion and deformation of the long target tube during subsequent machining and use. Moreover, the risk of cracking will increase due to reduced plasticity during straightening, resulting in product scrap. Conversely, if the temperature is too low, the atomic diffusion motive force will be insufficient, and complete metallurgical bonding of the interface will not be achieved. This will result in obvious traces or microscopic gaps at the joint of the target tube tube after machining, which will seriously affect the structural integrity and sputtering performance of the product and will also fail to meet the usage requirements.

[0038] Furthermore, if the pressure of the secondary hot isostatic pressing is too high, it will cause excessive plastic deformation of the tube blank, making it difficult to control dimensional accuracy. At the same time, it will keep the equipment under extreme load for a long time, increasing safety risks and maintenance costs. Conversely, if the pressure is too low, it will not provide enough driving force to promote atomic cross-interface diffusion and microscopic plastic rheology, resulting in insufficient bonding strength at the joints of segments. This will expose defects such as splicing marks, micro gaps, or even cracks during subsequent processing or use, seriously affecting the structural integrity and service reliability of the product.

[0039] According to a second aspect of the present invention, a molybdenum and / or molybdenum alloy tubular target prepared by the method described above is provided, which is composed of multiple pure molybdenum targets and / or multiple molybdenum alloy targets spliced ​​together.

[0040] Specifically, this invention allows for flexible adjustment of the target material composition according to design and requirements. The molybdenum alloy segment is precisely positioned in the critical sputtering area where a functional thin film needs to be deposited. Utilizing its excellent sputtering film-forming characteristics, the quality of the core film layer is ensured. Meanwhile, the pure molybdenum segment mainly serves as structural support, cooling conduction, or connection transition. Molybdenum alloys (such as molybdenum-titanium and molybdenum-niobium) have added expensive alloying elements, making their cost far higher than that of pure molybdenum. Using pure molybdenum segments in non-critical sputtering areas or in areas where there are no specific requirements for the thin film composition can significantly reduce the amount of expensive alloys used, thereby achieving significant raw material cost savings while ensuring the overall structural performance.

[0041] As an optional embodiment of the present invention, the molybdenum alloy target material includes one or more of the following: molybdenum-titanium alloy target material, molybdenum-titanium-nickel alloy target material, molybdenum-nickel alloy target material, molybdenum-titanium-niobium alloy target material, and molybdenum-niobium alloy target material.

[0042] Specifically, the present invention provides large-sized molybdenum and / or molybdenum alloy tubular targets with a length of 2.3 meters to 3.5 meters (e.g., 2.5 meters, 2.7 meters, 2.9 meters, 3.0 meters, 3.3 meters, etc.), and high density (≥99.5%) and oxygen content of 600-800 ppm (e.g., 650 ppm, 700 ppm, 750 ppm, etc.). The composition of the target can be flexibly adjusted according to design and requirements.

[0043] The present invention will now be described in further detail with reference to specific embodiments and comparative examples. Unless otherwise specified in the embodiments, conventional conditions or conditions recommended by the manufacturer shall apply.

[0044] Example 1 This embodiment provides a molybdenum-titanium alloy tubular target material, which is composed of three molybdenum-titanium alloy targets spliced ​​together.

[0045] This embodiment also provides a method for preparing the molybdenum-titanium alloy tubular target as described above, comprising the following steps: S1: Molybdenum powder with a purity of 99.95% and a Fisher particle size of 3.0μm and titanium powder with a purity of 99.6% and a mesh size of -300 are mixed at a mass ratio of 2:1 (this mass ratio is based on the existing molybdenum-titanium alloy model MT50). The mixture is mixed using a dual-motion mixer and argon gas is introduced to a pressure of 1.1 atmospheres. After mixing for 7 hours, a mixed powder is obtained. S2: The mixed powder is loaded into a tubular mold and subjected to cold isostatic pressing at a forming pressure of 200MPa for 15 minutes to form a tube blank. The tube blank is then shaped by a lathe with a forming size of D200 / 140×1000mm (outer diameter / inner diameter×length) to obtain a molybdenum-titanium alloy tubular compact. S3: Assemble the molybdenum-titanium alloy tubular blanks into three carbon steel sleeves, each sleeve measuring D210 / 130×1010mm (outer diameter / inner diameter×length). Perform vacuum degassing at 500℃ for 8 hours, maintaining a pressure of 10 kJ / kg inside the sleeves. -4 Pa, encapsulation welding seal; S4: The processed sheath is pressed in a hot isostatic pressing (HIP) machine at a temperature of 1100℃ and a pressure of 150MPa for 3 hours. After removing the sheath by machining, a molybdenum-titanium alloy tube is obtained with dimensions of D170 / 130×900mm (outer diameter / inner diameter×length) and a density of 94.5%. S5: The three sections of the molybdenum-titanium alloy tubing prepared above are spliced ​​and assembled along their length into a large-sized tubular sheath. The sheath dimensions are D175 / 125×2800mm (outer diameter / inner diameter×length). Vacuum degassing is performed at 550℃ for 6 hours, maintaining the pressure inside the sheath at 10... -4 Pa, encapsulation welding seal; S6: The large-size tube is encased in a hot isostatic pressing (HIP) machine and pressed at a temperature of 1200℃ and a pressure of 180MPa for 5 hours. After removing the encasing by machining, a molybdenum-titanium alloy tubular target is obtained with dimensions of D170 / 130×2700mm (outer diameter / inner diameter×length), a density of 99.9%, and an oxygen content of 700ppm.

[0046] Example 2 This embodiment provides a molybdenum-titanium-nickel alloy tubular target material, which is composed of four molybdenum-titanium-nickel alloy targets spliced ​​together.

[0047] This embodiment also provides a method for preparing the molybdenum-titanium-nickel alloy tubular target as described above, comprising the following steps: S1: Molybdenum powder with a purity of 99.95% and a Fisher particle size of 3.0μm, titanium powder with a purity of 99.6% and a -300 mesh, and nickel powder with a purity of 99% and a Fisher particle size of 4.5μm are mixed in a mass ratio of 7:2:1 (this mass ratio is based on the molybdenum-titanium-nickel alloy in patent TW 202035753 A). The mixture is mixed using a dual-motion mixer, and argon gas is introduced to a pressure of 1.2 atmospheres. After mixing for 6 hours, a mixed powder is obtained. S2: The mixed powder is loaded into a tubular mold and subjected to cold isostatic pressing at a forming pressure of 220MPa for 10 minutes to form a tube blank. The tube blank is then shaped by a lathe to a size of D220 / 150×800mm to obtain a molybdenum-titanium-nickel alloy tubular compact. S3: Assemble the molybdenum-titanium-nickel alloy tubular blanks into four carbon steel sleeves, each sleeve measuring D230 / 140×900mm (outer diameter / inner diameter×length). Perform vacuum evacuation at 550℃ for 6 hours, maintaining an internal pressure of 10... -4 Pa, encapsulation welding seal; S4: The processed sheath is pressed in a hot isostatic pressing (HIP) machine at a temperature of 1000℃ and a pressure of 150MPa for 4 hours. After removing the sheath by machining, a molybdenum-titanium-nickel alloy tube is obtained with dimensions of D190 / 140×650mm (outer diameter / inner diameter×length) and a density of 94.6%. S5: The four sections of the molybdenum-titanium-nickel alloy tubing prepared above are spliced ​​and assembled along the length to form a large-size tubular sheath with dimensions of D195 / 130×2700mm (outer diameter / inner diameter×length). A vacuum is then applied at 600℃ for 6 hours, maintaining an internal pressure of 10... -4 Pa, encapsulation welding seal; S6: The large-size tube is encased in a hot isostatic pressing (HIP) machine and pressed at a temperature of 1100℃ and a pressure of 180MPa for 6 hours. After removing the encasing by machining, a molybdenum-titanium-nickel alloy tubular target is obtained with dimensions of D180 / 140×2600mm (outer diameter / inner diameter×length), a density of 99.9%, and an oxygen content of 600ppm.

[0048] Example 3 This embodiment provides a molybdenum-niobium alloy tubular target material, which is composed of four molybdenum-niobium alloy targets spliced ​​together.

[0049] This embodiment also provides a method for preparing the molybdenum-niobium alloy tubular target as described above, comprising the following steps: S1: Molybdenum powder with a purity of 99.95% and a Fisher particle size of 3.2μm and niobium powder with a purity of 99.9% and a mesh size of -200 are mixed at a mass ratio of 9:1 (this mass ratio is based on the existing molybdenum-niobium alloy model MN10). The mixture is mixed using a dual-motion mixer and argon gas is introduced to a pressure of 1.1 atmospheres. After mixing for 6 hours, a mixed powder is obtained. S2: The mixed powder is loaded into a tubular mold and subjected to cold isostatic pressing at a forming pressure of 210MPa for 15 minutes to form a tube blank. The tube blank is then shaped by a lathe with a forming size of D200 / 140×900mm (outer diameter / inner diameter×length) to obtain a molybdenum-niobium alloy tubular compact. S3: Assemble the molybdenum-niobium alloy tubular blanks into four carbon steel sleeves, each sleeve measuring D210 / 130×1000mm (outer diameter / inner diameter×length). Perform vacuum evacuation at 600℃ for 6 hours, maintaining an internal pressure of 10... -4Pa, encapsulation welding seal; S4: The processed sheath is pressed in a hot isostatic pressing (HIP) machine at a temperature of 1200℃ and a pressure of 150MPa for 4 hours. After removing the sheath by machining, a molybdenum-niobium alloy tube is obtained with dimensions of D170 / 130×750mm (outer diameter / inner diameter×length) and a density of 94.2%. S5: The four sections of the molybdenum-niobium alloy tubing prepared above are spliced ​​and assembled along the length to form a large-size tubular sheath with dimensions of D175 / 125×3100mm (outer diameter / inner diameter×length). A vacuum is then applied at 600℃ for 6 hours, maintaining the air pressure inside the sheath at 10... -4 Pa, encapsulation welding seal; S6: The large-size tube is encased in a hot isostatic pressing (HIP) machine and pressed at a temperature of 1300℃ and a pressure of 180MPa for 5 hours. After removing the encasing by machining, a molybdenum-niobium alloy tubular target is obtained with dimensions of D170 / 130×3000mm (outer diameter / inner diameter×length), a density of 99.9%, and an oxygen content of 800ppm.

[0050] Example 4 This embodiment provides a molybdenum and molybdenum-titanium alloy tubular target, such as Figure 2 As shown, it is composed of two molybdenum targets and two molybdenum-titanium alloy targets, with the two molybdenum targets located at both ends of the tubular target.

[0051] This embodiment also provides a method for preparing the molybdenum and molybdenum-titanium alloy tubular target as described above, comprising the following steps: S1: Molybdenum powder with a purity of 99.95% and a Fisher particle size of 3.6μm and titanium powder with a purity of 99.9% and a mesh size of -200 are mixed at a mass ratio of 2:1 (this mass ratio is based on the existing molybdenum-titanium alloy MT50). The mixture is mixed using a dual-motion mixer and argon gas is introduced to a pressure of 1.1 atmospheres. After mixing for 5 hours, the mixed powder is obtained. S2: Molybdenum powder with a purity of 99.95% and a Fisher particle size of 3.6μm is loaded into a tubular mold and subjected to cold isostatic pressing at a forming pressure of 220MPa for 10 minutes to form a tube blank. The tube blank is then shaped by a lathe to a size of D220 / 150×400mm (outer diameter / inner diameter×length) to obtain a pure molybdenum tubular compact. The mixed powder is loaded into a tubular mold and subjected to cold isostatic pressing at a forming pressure of 200 MPa for 15 minutes to form a tube blank. The tube blank is then shaped by a lathe with a forming size of D220 / 150×1000 mm (outer diameter / inner diameter×length) to obtain a molybdenum-titanium alloy tubular compact. S3: The molybdenum-titanium alloy tubular compact and the pure molybdenum tubular compact are assembled in two carbon steel sleeves respectively. The sleeve dimensions for the molybdenum-titanium alloy tubular compact are D230 / 140×1100mm (outer diameter / inner diameter×length), and the sleeve dimensions for the pure molybdenum tubular compact are D230 / 140×500mm (outer diameter / inner diameter×length). Both are subjected to vacuuming at 550℃ for 7 hours, maintaining the air pressure inside the sleeve at 10. -4 Pa, encapsulation welding seal; S4: The two processed sheaths are pressed in a hot isostatic pressing (HIP) machine at a temperature of 1100℃ and a pressure of 150MPa for 3 hours. After removing the sheaths by machining, pure molybdenum tubing and molybdenum-titanium alloy tubing are obtained. The pure molybdenum tubing has dimensions of D180 / 140×300mm and a density of 94.2%. The molybdenum-titanium alloy tubing has dimensions of D180 / 140×900mm (outer diameter / inner diameter×length) and a density of 94.5%. S5: Insert the pure molybdenum tube, two molybdenum-titanium alloy tubes, and the pure molybdenum tube sequentially along their length into a large-size tube sheath. The large-size tube sheath measures D185 / 135×2500mm (outer diameter / inner diameter×length). Perform a vacuum test at 500℃ for 6 hours, maintaining a pressure of 10 kJ / kg inside the sheath. -4 Pa, encapsulation welding seal; S6: The large-size tube is encased in a hot isostatic pressing (HIP) machine and pressed at a temperature of 1200℃ and a pressure of 180MPa for 5 hours. After removing the encasing by machining, a molybdenum-niobium alloy tubular target is obtained with dimensions of D175 / 130×2300mm (outer diameter / inner diameter×length), a density of 99.9%, and an oxygen content of 600ppm.

[0052] Comparative Example 1 The difference between this comparative example and Example 1 is that, in step S1, argon gas is not introduced during the powder mixing process, and the gas pressure is 1 atmosphere. The remaining steps and technical parameters are the same as those in Example 1.

[0053] The molybdenum-titanium alloy tubular target prepared in Comparative Example 1 has a density of 99.8% and an oxygen content of 1500 ppm.

[0054] Comparative Example 2 The difference between this comparative example and Example 1 is that steps S5 and S6 are omitted, that is, hot isostatic pressing is performed only once, specifically including the following steps: S3: Assemble the three-section molybdenum-titanium alloy tubular blanks obtained in step S2 of Example 1 along their length into a large-sized carbon steel sheath. The sheath dimensions are D210 / 130×3010mm (outer diameter / inner diameter×length). Perform vacuum degassing at 500℃ for 8 hours, maintaining the gas pressure inside the sheath at 10... -4 Pa, encapsulation welding seal; S4: The processed sheath is pressed in a hot isostatic pressing (HIP) machine at a temperature of 1100℃ and a pressure of 150MPa for 3 hours. After removing the sheath by machining, a molybdenum-titanium alloy tube is obtained with dimensions of D170 / 130×2500mm (outer diameter / inner diameter×length) and a density of 95%. The remaining steps and technical parameters are the same as in Example 1.

[0055] The molybdenum-titanium alloy tubular target in this comparative example was too long. After being packaged, it underwent a hot isostatic pressing. Under gravity, high temperature and high pressure, the compact shrank unevenly, and the middle part bent. This resulted in the middle part being smaller than expected, and the pass rate (the pass criterion is that the final product meets the preset product size) dropped to 50%.

[0056] Furthermore, through extensive experiments, the inventors discovered that when the molybdenum-titanium alloy tubular blanks obtained in step S2 of Example 1 are first sintered at high temperature, and then multiple sintered tubular blanks are assembled along their length into a large-sized carbon steel sheath, and steps S3 and S4 of this comparative example are performed, the resulting molybdenum-titanium alloy tubular target material also has similar problems to that of this comparative example. That is, the large-sized blanks shrink inconsistently under gravity, high temperature, and high pressure, causing the middle part to bend. Subsequent straightening and adjustment, as well as annealing of the bent parts, are required. The preparation method is complex, and the annealing treatment can also lead to coarse grains in the bent parts, affecting the reliability of the final product.

[0057] The present invention assembles multiple sections of molybdenum and / or molybdenum alloy tubing into a large-size tubular sheath and performs secondary hot isostatic pressing. This not only enables the joints of the multiple sections of tubing to have high density, significantly improving the strength and structural integrity of the target material, but also eliminates the need for complex straightening and trimming processes, thereby improving production efficiency and reducing the high scrap rate and huge processing costs associated with large-scale integral forging or sintering.

[0058] Comparative Example 3 The difference between this comparative example and Example 1 is that in step S6, the temperature of the secondary hot isostatic pressing is 800°C, while the remaining steps and technical parameters are the same as in Example 1.

[0059] The molybdenum-titanium alloy tubular target obtained in step S6 has a density of 97.2%.

[0060] The molybdenum-titanium alloy tubular target prepared in this comparative example, such as Figure 3 As shown, there are obvious marks at the joint of the tube target after machining, and there are gaps in the fit, making it impossible to process it into the preset product size, and the product is unqualified.

[0061] Comparative Example 4 The difference between this comparative example and Example 1 is that in step S6, the temperature of the secondary hot isostatic pressing is 1300°C, while the remaining steps and technical parameters are the same as in Example 1.

[0062] The molybdenum-titanium alloy tubular target obtained in step S6 has a density of 98.1%.

[0063] In this comparative example, after the molybdenum-titanium alloy tubular target was removed by machining in step S6, it was found that the tubular target showed local softening, the long tubular target was deformed and twisted, and it was prone to cracking when straightening, resulting in unqualified products.

[0064] Comparative Example 5 The difference between this comparative example and Example 1 is that in step S6, the pressure of the secondary hot isostatic pressing is 200 MPa, while the remaining steps and technical parameters are the same as in Example 1.

[0065] The molybdenum-titanium alloy tubular target obtained in step S6 has a density of 98.5%.

[0066] In this comparative example, the excessive pressure during the secondary hot isostatic pressing caused excessive plastic deformation of the tube blank, making it impossible to process into the preset product size, resulting in a substandard product.

[0067] Comparative Example 6 The difference between this comparative example and Example 1 is that in step S6, the pressure of the secondary hot isostatic pressing is 140 MPa, while the remaining steps and technical parameters are the same as in Example 1.

[0068] The molybdenum-titanium alloy tubular target obtained in step S6 has a density of 98%.

[0069] In this comparative example, the pressure of the secondary hot isostatic pressing was too low, resulting in insufficient bonding strength at the joint of the segments. This caused gaps at the joints, making it impossible to process the product to the preset dimensions, and the product was unqualified.

[0070] Comparative Example 7 The difference between this comparative example and Example 1 is that in step S4, the temperature of the first hot isostatic pressing is 700°C, while the remaining steps and technical parameters are the same as in Example 1.

[0071] In this comparative example, the density of the molybdenum-titanium alloy tube prepared in step S4 was low (91%) due to the low temperature of the first hot isostatic pressing. Furthermore, after the second hot isostatic pressing, it could not be processed into the preset product size, resulting in a defective product.

[0072] Comparative Example 8 The difference between this comparative example and Example 1 is that in step S4, the temperature of the first hot isostatic pressing is 1300°C, while the remaining steps and technical parameters are the same as in Example 1.

[0073] The density of the molybdenum-titanium alloy tube obtained in step S4 is 92.5%.

[0074] In this comparative example, the strength and toughness of the molybdenum-titanium alloy pipe prepared in step S4 were significantly reduced due to the excessively high temperature of the first hot isostatic pressing, resulting in partial softening of the pipe and making it impossible to undergo a second hot isostatic pressing treatment.

[0075] Comparative Example 9 The difference between this comparative example and Example 1 is that in step S4, the pressure of the first hot isostatic pressing is 180 MPa, while the remaining steps and technical parameters are the same as in Example 1.

[0076] The density of the molybdenum-titanium alloy tube obtained in step S4 is 95.5%.

[0077] In this comparative example, the molybdenum-titanium alloy tube prepared in step S4 was severely out of dimensional and had micro-cracks due to excessively high pressure during the first hot isostatic pressing process, making it impossible to perform a second hot isostatic pressing.

[0078] Comparative Example 10 The difference between this comparative example and Example 1 is that in step S4, the pressure of the first hot isostatic pressing is 80 MPa, while the remaining steps and technical parameters are the same as in Example 1.

[0079] In this comparative example, the pressure of the first hot isostatic pressing was too low, resulting in porosity in the molybdenum-titanium alloy tube prepared in step S4. Consequently, the density of the molybdenum-titanium alloy tube prepared in step S4 was low, at 90%. Furthermore, after the second hot isostatic pressing treatment, it could not be processed into the preset product size, and the product was unqualified.

[0080] Comparative Example 11 The main difference between this comparative example and Example 1 is that the time, pressure and duration of the secondary hot isostatic pressing in step S6 are the same as those of the primary hot isostatic pressing in step S4, while the remaining steps and technical parameters are consistent with those of Example 1.

[0081] In this comparative example, since the temperature, pressure and time of the second hot isostatic pressing are the same as those of the first hot isostatic pressing, the atomic diffusion kinetic energy in the billet is insufficient, which prevents sufficient plastic rheology from occurring at the micro protrusions at the interface to achieve a tight fit. After machining, obvious traces are visible at the joint, reducing the density of the target material to 98.5%.

[0082] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A method for preparing a tubular target material of molybdenum and / or molybdenum alloy, characterized in that, Includes the following steps: S1: Provide molybdenum powder and / or molybdenum alloy powder; S2: Molybdenum powder and / or molybdenum alloy powder are cold isostatically pressed to obtain a tube blank, and then the tube blank is shaped to obtain a pure molybdenum tubular compact and / or a molybdenum alloy tubular compact. S3: Assemble one or more sections of pure molybdenum tubular blanks and / or molybdenum alloy tubular blanks in a cladding, and then degas and seal the cladding. S4: After the degassing and sealing of the casing, hot isostatic pressing is performed, and the casing is removed by machining to obtain pure molybdenum pipe and / or molybdenum alloy pipe; S5: Reassemble at least two sections of pure molybdenum pipe and / or molybdenum alloy pipe into a large-size pipe sheath, and then degas and seal the large-size pipe sheath. S6: After degassing and sealing, the large-size tubular casing is subjected to secondary hot isostatic pressing, and the casing is removed by machining to obtain a molybdenum and / or molybdenum alloy tubular target.

2. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 1, characterized in that, The Fisher particle size of molybdenum powder is 2.5~4.5μm; And / or, molybdenum alloy powder includes molybdenum powder and alloy powder; Alloy powders include one or more of titanium powder, nickel powder, and niobium powder; The particle size of both titanium powder and niobium powder is 325 mesh to -200 mesh; The Fisher particle size of nickel powder is 3~5μm; The purity of both molybdenum powder and alloy powder is greater than 99%.

3. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 2, characterized in that, In step S1, the method for preparing the molybdenum alloy powder includes: mixing molybdenum powder and alloy powder using a dual-motion mixer, introducing a protective gas during the mixing process at a pressure of 1.1-1.2 atmospheres, and mixing for 4-10 hours. The protective gas is argon, nitrogen, or helium.

4. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 1, characterized in that, In step S2, molybdenum powder and / or molybdenum alloy powder are loaded into a tubular mold and subjected to cold isostatic pressing. The pressure of the cold isostatic pressing is 200-250 MPa, and the holding time is 5-15 min. And / or, in step S2, the shaping process refers to shaping through machining.

5. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 1, characterized in that, In step S3, the degassing of the cladding involves vacuuming the cladding at 500-600℃ for 6-10 hours until the gas pressure inside the cladding is ≤10. -4 Pa.

6. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 1, characterized in that, In step S4, the conditions for a single hot isostatic pressing include: Temperature: 850-1450℃; Pressure: 100-150MPa; Time: 1-6h; Specifically, when the molybdenum alloy pipe is a molybdenum-titanium alloy pipe, a molybdenum-titanium-nickel alloy pipe, or a molybdenum-nickel alloy pipe, the conditions for a single hot isostatic pressing include: a temperature of 900-1200℃, a pressure of 100-150MPa, and a time of 1-6h. When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for a single hot isostatic pressing include: temperature of 1200-1450℃, pressure of 100-150MPa, and time of 1-6h. When the pipe is pure molybdenum, the conditions for a single hot isostatic pressing include: temperature of 900-1200℃, pressure of 100-150MPa, and time of 1-6h. And / or, in step S4, the density of the obtained pure molybdenum tubing and / or molybdenum alloy tubing is ≥94.5%.

7. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to claim 1, characterized in that, In step S5, the large-size pipe sheathing refers to assembling and splicing multiple sections of pure molybdenum pipe and / or multiple sections of molybdenum alloy pipe together, and then sheathing them. And / or, the length of the combined pipe in the large-size pipe sheath is 2.3 meters to 3.5 meters; And / or, degassing of large-size tube sheaths involves vacuum degassing of the large-size tube sheath at 500-600℃ for 6-10 hours until the gas pressure inside the sheath is ≤10. -4 Pa.

8. The method for preparing the molybdenum and / or molybdenum alloy tubular target according to any one of claims 1 or 6, characterized in that, In step S6, the conditions for secondary hot isostatic pressing include: Temperature: 950-1550℃; Pressure: 160-180MPa; Time: 3-10h; Specifically, when the molybdenum alloy pipe is a molybdenum-titanium alloy pipe, a molybdenum-titanium-nickel alloy pipe, or a molybdenum-nickel alloy pipe, the conditions for secondary hot isostatic pressing include: 950-1200℃, pressure of 160-180MPa, and time of 3-10h. When the molybdenum alloy pipe is a molybdenum-niobium alloy pipe, the conditions for secondary hot isostatic pressing include: temperature of 1200-1550℃, pressure of 160-180MPa, and time of 3-10h. When the tubing is pure molybdenum, the conditions for secondary hot isostatic pressing include: 950-1200℃, pressure of 160-180MPa, and time of 3-10h. And / or, the temperature, pressure, and time of the secondary hot isostatic pressing are all greater than those of the primary hot isostatic pressing.

9. A molybdenum and / or molybdenum alloy tubular target prepared by the method for preparing a molybdenum and / or molybdenum alloy tubular target as described in any one of claims 1-8, characterized in that, It is composed of multiple pure molybdenum targets and / or multiple molybdenum alloy targets spliced ​​together.

10. The molybdenum and / or molybdenum alloy tubular target according to claim 9, characterized in that, The molybdenum alloy target material includes one or more of the following: molybdenum-titanium alloy target material, molybdenum-titanium-nickel alloy target material, molybdenum-nickel alloy target material, molybdenum-titanium-niobium alloy target material, and molybdenum-niobium alloy target material. And / or, the length of the molybdenum and / or molybdenum alloy tubular target is 2.3 meters to 3.5 meters; And / or, the density of the molybdenum and / or molybdenum alloy tubular target is ≥99.5%; And / or, the oxygen content of the molybdenum and / or molybdenum alloy tubular target is 600-800 ppm.

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