A method for preparing a Mo-ZrN dual-phase composite target material by hot isostatic pressing and application thereof

Abstract

The application belongs to the technical field of powder metallurgy, and particularly relates to a method for preparing Mo-ZrN dual-phase composite target material through hot isostatic pressing, which comprises the following steps: firstly, Mo powder and ZrN powder are subjected to cold isostatic pressing, sintering, first hot isostatic pressing and first annealing processes in sequence to obtain Mo target blanks and ZrN target blanks; then, the Mo target blanks and the ZrN target blanks are pretreated, a (Ti+TiN) transition layer is filled between the Mo target blanks and the ZrN target blanks, a composite blank is obtained, and then heating, sealing, second hot isostatic pressing and post-processing are sequentially performed to finally obtain the Mo-ZrN dual-phase composite target material. Through the introduction of the (Ti+TiN) transition layer material and the matching of the corresponding hot isostatic pressing process parameters, the diffusion connection of Mo and ZrN is realized, and finally the sputtering stability and the film deposition quality of the Mo-ZrN dual-phase composite target material are improved.

Description

Technical Field

[0001] This invention belongs to the field of powder metallurgy technology, and relates to a method for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing and its application. Background Technology

[0002] With the widespread adoption of high-power sputtering technology, the requirements for sputtering target density, backplane heat dissipation performance, and target-backplane bonding processes are becoming increasingly stringent. Molybdenum (Mo) targets possess excellent high-temperature structural and performance stability, along with high electrical and thermal conductivity, making them suitable for fabricating functional components such as electrodes, back electrodes, and heating layers. Zirconium nitride (ZrN) targets combine the electrical conductivity of metals with the high hardness and wear resistance of nitrides, making them ideal materials for depositing decorative and functional hard films. Therefore, combining the highly conductive and thermally conductive Mo target with the high-hardness and highly functional ZrN target allows the target to simultaneously meet the heat dissipation requirements and functional phase supply needs in high-power sputtering scenarios, thereby supporting higher line power sputtering processes and achieving more stable thin film deposition results.

[0003] Currently, the mainstream preparation methods for dual-phase composite sputtering targets are mechanical splicing and bonding processes, specifically including mechanical slot fixing, indium-based bonding, elastic bonding, and diffusion bonding. However, these methods generally suffer from the following technical defects: the target interface is prone to peeling, delamination, or detachment; excessively high local contact resistance at the interface can easily lead to local overheating, resulting in strong arcs during sputtering; target particle detachment can easily cause film contamination; thermal cycling fatigue can easily induce cracks in the target or bonding layer, ultimately leading to bonding failure. Furthermore, bonding materials or adhesives are prone to decomposition and volatilization under vacuum and high-temperature sputtering environments, further contaminating the deposited film; and mechanical loosening or relative slippage can easily occur between the target and the backing plate due to vibration or mismatch in thermal expansion coefficients.

[0004] Therefore, there is an urgent need to propose a method for preparing Mo-ZrN dual-phase composite targets to solve the above-mentioned technical problems. Summary of the Invention

[0005] The purpose of this invention is to overcome the shortcomings of the prior art and propose a method for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing (HIP) and its application. This method introduces a (Ti+TiN) transition layer material between the Mo and ZrN target blanks, and, in conjunction with appropriate HIP process parameters, achieves metallurgical diffusion bonding between the Mo and ZrN target blanks. This method improves the interfacial bonding strength of the Mo-ZrN dual-phase composite target, enhances its electrical conductivity and thermal matching performance, and improves the sputtering stability and thin film deposition quality of the Mo-ZrN dual-phase composite target.

[0006] To achieve the above objectives, the present invention provides the following technical solution: In a first aspect, the present invention provides a method for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing, comprising the following steps: S1. Mo powder and ZrN powder are subjected to cold isostatic pressing, sintering, first hot isostatic pressing and first annealing respectively to obtain Mo target blank and ZrN target blank. S2. The Mo target blank and ZrN target blank are pretreated respectively, and then a transition layer is filled between them to obtain a composite blank. The composite blank is placed in a sleeve, and then subjected to staged heating, sealing and welding and a second hot isostatic pressing to obtain a Mo-ZrN dual-phase composite target blank. The Mo-ZrN dual-phase composite target blank is post-treated to finally obtain the Mo-ZrN dual-phase composite target material.

[0007] Specifically, in S1, both the Mo powder and ZrN powder need to be homogenized by mechanical ball milling before cold isostatic pressing.

[0008] Specifically, in S2, the material of the sheath includes, but is not limited to, 20# steel, 45# steel, 304 stainless steel or pure titanium (CP-Ti).

[0009] More specifically, the cladding is preferably made of 20# steel or 45# steel, because both 20# steel and 45# steel are carbon steels, which are not only inexpensive but also have excellent plastic deformation capabilities during hot isostatic pressing.

[0010] Specifically, in S2, the staged heating operation preferably uses a resistance heating furnace.

[0011] Specifically, in S2, the sealing operation involves the following steps: vacuuming the sheath, simultaneously flattening the degassing tube of the sheath using specialized pliers, breaking the degassing tube, and then performing electron beam welding for sealing. After sealing, the vacuum level inside the sheath must be less than 10. -4 Pa.

[0012] Furthermore, in S1, the particle size of both the Mo powder and the ZrN powder is 1~10μm, the purity is 99.90%~99.95%, and the oxygen content, nitrogen content, and carbon content are all no more than 50 ppm. Further, in S1, the pressure of the cold isostatic pressing is 200~400MPa, and the holding time is 5~15min; the temperature of the sintering process is 1500~2000℃, and the time is 2~4h; the pressure of the first hot isostatic pressing is 150~200MPa, the holding time is 2~5h, and the temperature is 1500~1800°C; the holding temperature of the first annealing is 1000~1400℃, and the holding time is 1~4h.

[0013] Specifically, the cold isostatic pressing is performed at room temperature.

[0014] Specifically, the sintering process is carried out under vacuum, with a vacuum degree of 10. -3 Pa~10 -2 Pa.

[0015] Specifically, the first annealing is performed under vacuum, with a vacuum level of 10. -5 ~10 -3 Pa is used to eliminate the residual stress in the Mo and ZrN target blanks.

[0016] Furthermore, in S2, the pretreatment sequentially includes grinding, polishing, and cleaning; after pretreatment, the surface roughness of the Mo target blank and the ZrN target blank is ≤0.8μm, and the flatness is <0.05 mm.

[0017] Specifically, the grinding process involves fixing the Mo and ZrN target blanks onto the worktable of a precision surface grinder; first, rough grinding is performed using a diamond grinding wheel with a grit size of 80-120 mesh; then, semi-finish grinding is performed using a diamond grinding wheel with a grit size of 200-400 mesh; finally, fine grinding is performed using a diamond grinding wheel with a grit size of 600-1000 mesh. Subsequently, the finely ground Mo and ZrN target blanks are cleaned using ultrasonic cleaning, and after cleaning, they are placed in a vacuum drying oven to dry (at a temperature of 60°C).

[0018] Specifically, the polishing process involves the following steps: fixing the ground Mo and ZrN target blanks onto the working disc of a surface polishing machine; first, using diamond polishing paste with a particle size of 3-6 μm to remove residual texture from the grinding process; then, polishing with diamond polishing slurry with a particle size of 1 μm to reduce the surface roughness of both the Mo and ZrN target blanks to Ra≤0.5 μm; finally, polishing with alumina suspension or colloidal silica polishing slurry with a particle size of 0.05 μm to reduce the surface roughness of both the Mo and ZrN target blanks to Ra≤0.3 μm; subsequently, cleaning with anhydrous ethanol and drying in a vacuum drying oven (at 60°C).

[0019] Specifically, the purpose of the cleaning process is to remove residual oil and polishing paste from the processing. The specific steps are as follows: ultrasonic cleaning is performed on the polished Mo target blank and ZrN target blank respectively. The ultrasonic cleaning frequency is 20~40kHz and the cleaning time is 5~15min.

[0020] Furthermore, in S2, the staged heating includes a low-temperature heating stage and a high-temperature heating stage. The temperature of the low-temperature heating stage is 200~230°C, and the holding time is 2~5h. The temperature of the high-temperature heating stage is 380~430°C, and the holding time is 2~5h. The temperature of the second hot isostatic pressing is 1200~1400°C, the pressure is 20~50MPa, and the holding time is 2~5h.

[0021] Furthermore, in S1, the thickness ratio of the Mo target blank to the ZrN target blank is 1:1.

[0022] Furthermore, in S2, the transition layer is made of Ti and TiN dual-phase materials, with the thickness of Ti material being 5~20µm and the thickness of TiN material being 5~10µm.

[0023] Further, in S2, the post-processing operation includes a second annealing, cutting, and polishing in sequence; the holding temperature of the second annealing is 1000~1100℃, and the holding time is 1~2h; after polishing, the surface roughness Ra of the Mo-ZrN dual-phase composite target material is <0.5μm.

[0024] Specifically, the second annealing is performed under vacuum, with a vacuum level of 10. -5 ~10 -3 Pa.

[0025] Specifically, the cutting process preferably uses laser cutting to process the Mo-ZrN dual-phase composite target blank into a specific shape and size.

[0026] Secondly, the present invention discloses any of the above-mentioned methods for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing, which can be used in wear-resistant coatings, decorative coatings, and protective layers for electronic devices.

[0027] Compared with the prior art, the present invention has the following beneficial effects: First, Mo-ZrN belongs to a metal (Mo) + ceramic (ZrN) dual-phase system. This combination is a metal-ceramic coupling, with significant differences in thermal, electrical, and mechanical properties. Interface reaction, embrittlement, and mismatch in thermal expansion coefficients are the main challenges. This invention sets a (Ti+TiN) composite transition layer material between the Mo and ZrN target blanks, which have significantly different thermal expansion coefficients, and adopts compatible hot isostatic pressing process parameters. This effectively alleviates the problem of thermal expansion coefficient mismatch between Mo and ZrN, reduces stress concentration at the interface, and not only increases the interfacial shear strength of the dual-phase composite target to over 200 MPa, achieving a strong and reliable interface bond, but also reduces the interfacial contact resistance by forming a good conductive path between the transition layer and the substrate, increasing the overall conductivity of the target material by about 30%, which helps stabilize arc ignition and discharge during sputtering. Simultaneously, the number of arc discharges during sputtering is reduced by more than 90%, improving film quality and stability, and increasing the film deposition rate by about 40% under the same process conditions, thereby achieving cost reduction and efficiency improvement.

[0028] Secondly, the material system determines the possibility of interfacial chemical reactions, the temperature and pressure window of hot isostatic pressing (HIP), and key design variables such as electrical conductivity, thermal conductivity, and arc-start risk during sputtering. Compared to the "mono-target" process used in metallurgical bonding of homogeneous materials, this invention innovatively adopts a "(Ti + TiN) transition layer + cladding seal + HIP diffusion bonding" process. The aim is to achieve a reliable interface for metallurgical diffusion bonding, mitigate differences in thermal expansion coefficients, and ensure high thermal and electrical conductivity (suitable for high-power sputtering). This process solves the problem of mismatch between the interfacial bonding and thermal expansion coefficients of Mo and ZrN ceramics during HIP. The interfacial reaction control and diffusion bonding regulation strategy adopted in this invention represents a new application of powder metallurgy HIP technology in the field of metal / ceramic dual-phase composite targets.

[0029] Third, after thermal cycling testing, the target interface remains intact and stable, without cracking, delamination, or loosening, significantly extending the target's service life and process adaptability. This achieves a comprehensive improvement in the interface bonding strength, thermoelectric stability, sputtering stability, and film deposition uniformity of the dual-phase composite target, solving the technical problems of short service life, poor film quality, and low production efficiency caused by weak interface bonding and unstable performance of Mo-ZrN dual-phase composite targets in the prior art. Attached Figure Description

[0030] The accompanying drawings are incorporated in and form part of this specification, and together with the description serve to explain the principles of the invention.

[0031] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0032] Figure 1 This is a flowchart illustrating the preparation process of the present invention. Detailed Implementation

[0033] Exemplary embodiments will now be described in detail. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples consistent with some aspects of the invention as detailed in the appended claims.

[0034] To enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments.

[0035] Example 1 like Figure 1As shown, this embodiment provides a method for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing, including the following steps: S1. Weigh out Mo powder and ZrN powder with a particle size of 1μm and a purity of 99.90%, respectively. After homogenization by ball milling, perform cold isostatic pressing, sintering, first hot isostatic pressing and first annealing processes in sequence to obtain Mo target blank and ZrN target blank. The thickness ratio of the Mo target blank and ZrN target blank is 1:1.

[0036] Specifically, the cold isostatic pressing is performed at room temperature, with a pressure of 200 MPa and a holding time of 15 min.

[0037] Specifically, the vacuum degree of the sintering process is 10. -3 Pa, temperature 1500℃, time 4h.

[0038] Specifically, the pressure of the first hot isostatic pressing is 150 MPa, the holding time is 5 hours, and the temperature is 1500℃.

[0039] The vacuum degree of the first annealing is 10. -3 Pa, the heat preservation temperature is 1000℃, and the heat preservation time is 4h.

[0040] S2. Grind the Mo target blank and ZrN target blank separately and fix them on the worktable of a precision surface grinder; use a 100-mesh diamond grinding wheel for rough grinding, then use a 300-mesh diamond grinding wheel for semi-finish grinding, and finally use an 800-mesh diamond grinding wheel for finish grinding; then, use ultrasonic cleaning to clean the finely ground Mo target blank and ZrN target blank. After cleaning, place the finely ground Mo target blank and ZrN target blank in a vacuum drying oven to dry (drying temperature is 60℃).

[0041] Subsequently, the ground Mo and ZrN target blanks were fixed on the working disc of a surface polishing machine. First, diamond polishing paste with a particle size of 3 μm was used to remove residual texture from the grinding process. Then, diamond polishing slurry with a particle size of 1 μm was used for polishing, reducing the surface roughness of both the Mo and ZrN target blanks to Ra≤0.5 μm. Finally, alumina suspension or colloidal silica polishing slurry with a particle size of 0.05 μm was used for polishing, reducing the surface roughness of both the Mo and ZrN target blanks to Ra≤0.3 μm. Finally, the polished Mo and ZrN target blanks were cleaned with anhydrous ethanol and dried in a vacuum drying oven (at a temperature of 60°C).

[0042] Next, the polished Mo target blank and ZrN target blank were subjected to ultrasonic cleaning at a frequency of 30 kHz for 10 min. After the pretreatment process, the surface roughness of the Mo target blank and ZrN target blank was ≤0.8 μm and the flatness was <0.05 mm.

[0043] Ti foil and TiN foil, both with a thickness of 5 µm, were selected as filler transition layer materials and filled between the pretreated Mo target blank and ZrN target blank to obtain a composite blank. The composite blank was placed in a 20# steel sleeve and then subjected to staged heating, sealing welding and a second hot isostatic pressing to obtain a Mo-ZrN dual-phase composite target blank. The Mo-ZrN dual-phase composite target blank was post-processed to finally obtain the Mo-ZrN dual-phase composite target material.

[0044] Specifically, in the staged heating process, the temperature of the low-temperature heating stage is 200℃ and the time is 2h; the temperature of the high-temperature heating stage is 380℃ and the time is 2h.

[0045] Specifically, the second hot isostatic pressing is performed at a pressure of 50 MPa, a temperature of 1200℃, and a holding time of 5 hours.

[0046] Specifically, the post-processing includes a second annealing, cutting, and polishing in sequence.

[0047] More specifically, the vacuum degree of the second annealing is 10. -3 Pa, the heat preservation temperature is 1000℃, and the heat preservation time is 2h.

[0048] More specifically, after polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.48 μm.

[0049] Example 2 The preparation method in this embodiment is the same as that in Example 1, except that: In S1: The Mo powder and ZrN powder both have a particle size of 5 μm and a purity of 99.93%.

[0050] The cold isostatic pressing pressure is 300 MPa, and the time is 10 min; The vacuum degree of the sintering is 10. -4 Pa, temperature 1700℃, time 3h; The first hot isostatic pressing was performed at a pressure of 170 MPa, a temperature of 1650℃, and a holding time of 3 h. The vacuum degree of the first annealing is 10. -4 Pa, the heat preservation temperature is 1200℃, and the heat preservation time is 2h.

[0051] In S2: During the grinding process, an 80-mesh diamond grinding wheel is used for rough grinding, a 200-mesh diamond grinding wheel is used for semi-finish grinding, and a 600-mesh diamond grinding wheel is used for finish grinding. During the polishing process, diamond polishing paste with a particle size of 4μm is used to remove residual texture from the grinding process; During the cleaning process, the ultrasonic cleaning frequency is 40 kHz and the cleaning time is 5 min; The filling transition layer material is composed of 10µm Ti material and 8µm TiN material; The sheath is made of 45# steel; In the staged heating process, the temperature of the low-temperature heating stage is 210℃ and the time is 3 hours; the temperature of the high-temperature heating stage is 400℃ and the time is 4 hours. The second hot isostatic pressing was performed at a pressure of 40 MPa, a temperature of 1300℃, and a holding time of 3 h. The vacuum degree of the second annealing is 10. -4 Pa, the heat preservation temperature is 1050℃, and the time is 1.5 h; After polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.42 μm.

[0052] Example 3 The preparation method in this embodiment is the same as that in Example 1, except that: In S1: The Mo powder and ZrN powder both have a particle size of 10 μm and a purity of 99.95%. The cold isostatic pressing pressure is 400 MPa, and the time is 5 min; The vacuum degree of the sintering is 10. -5 Pa, temperature 2000℃, time 2 h; The first hot isostatic pressing was performed at a pressure of 200 MPa, a temperature of 1800℃, and a holding time of 2 h. The vacuum degree of the first annealing is 10. -5 Pa, the heat preservation temperature is 1400℃, and the heat preservation time is 1h.

[0053] In S2: During the grinding process, a diamond grinding wheel with a grit size of 120 mesh is used for rough grinding, a diamond grinding wheel with a grit size of 400 mesh is used for semi-finish grinding, and a diamond grinding wheel with a grit size of 1000 mesh is used for finish grinding. During the polishing process, diamond polishing paste with a particle size of 6μm is used to remove residual texture from the grinding process; During the cleaning process, the ultrasonic cleaning frequency is 20 kHz and the cleaning time is 15 min; The filling transition layer material is composed of 20 µm Ti material and 10 µm TiN material; The sheath is made of 45# steel; In the staged heating process, the temperature of the low-temperature heating stage is 230℃ and the time is 5 hours; the temperature of the high-temperature heating stage is 430℃ and the time is 5 hours. The second hot isostatic pressing was performed at a pressure of 20 MPa, a temperature of 1400℃, and a holding time of 2 h. The vacuum degree of the second annealing is 10. -5 Pa, the heat preservation temperature is 1100℃, and the time is 1 h; After polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.45 μm.

[0054] Comparative Example 1 The preparation method in this embodiment is the same as that in Example 2, except that: After the Mo target blank and ZrN target blank are pretreated, no transition layer material is filled between them; After polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.41 μm.

[0055] Comparative Example 2 The preparation method in this embodiment is the same as that in Example 2, except that: After the Mo target blank and ZrN target blank are pretreated, no transition layer material is filled between them; The Mo target blank and the ZrN target blank are fixedly connected by a mechanical slot to replace the heating, sealing and hot isostatic pressing process in step S2 of embodiment 2. After polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.42 μm.

[0056] Comparative Example 3 The preparation method in this embodiment is the same as that in Example 2, except that: The first hot isostatic pressing was performed at a pressure of 100 MPa, a temperature of 1300℃, and a holding time of 3 hours. After polishing, the surface roughness of the Mo-ZrN dual-phase composite target is 0.43 μm.

[0057] In addition, the performance test results of the Mo-ZrN biphase composite targets prepared in Examples 1-3 and Comparative Examples 1-3 are shown in Table 1.

[0058] Table 1 Properties of Mo-ZrN Dual-Phase Composite Targets As shown in Table 1, the Mo-ZrN dual-phase composite targets prepared in Examples 1-3 are significantly superior to those in Comparative Examples 1-3 in key indicators such as relative density, interfacial shear strength, electrical conductivity, sputtering stability, and thermal cycling reliability, exhibiting better overall performance, as detailed below: The Mo-ZrN biphase composite targets prepared in Examples 1-3 had relative densities of 99.1%, 99.8%, and 99.7%, respectively, all of which were close to being completely dense; while the relative densities of Comparative Examples 1-3 were only 97.5%, 96.8%, and 95.2%, respectively, indicating that there were non-dense defects inside the targets.

[0059] The Mo-ZrN biphase composite targets prepared in Examples 1-3 had interfacial shear strengths of 185 MPa, 235 MPa, and 228 MPa, respectively, indicating that a high-strength metallurgical bond was formed between Mo and ZrN and the interfacial bond was strong. In contrast, the interfacial shear strengths of Comparative Examples 1-3 were only 82 MPa, 65 MPa, and 110 MPa, respectively, indicating that the interfacial bond was significantly insufficient.

[0060] The Mo-ZrN biphase composite targets prepared in Examples 1-3 have electrical conductivity of 42% IACS, 46% IACS, and 45% IACS, respectively, maintaining a high level. In contrast, the electrical conductivity of Comparative Examples 1-3 is only 38% IACS, 35% IACS, and 33% IACS. The lower the electrical conductivity of the target material, the worse its conductivity, which can easily cause uneven current distribution during sputtering, leading to decreased sputtering stability and increased arcing.

[0061] The Mo-ZrN dual-phase composite targets prepared in Examples 1-3 exhibited sputtering rates of 52 nm / min, 58 nm / min, and 56 nm / min, respectively, demonstrating higher overall sputtering rates and superior film deposition efficiency. Simultaneously, the arc counts were 1 / h, 0 / h, and 0 / h, respectively, indicating virtually no arc generation and a stable and reliable sputtering process. Furthermore, the film thickness uniformity was ±3.2%, ±2.1%, and ±2.5%, respectively, showing minimal film thickness fluctuations and good film consistency. In contrast, the sputtering rates of Comparative Examples 1-3 were only 41 nm / min, 37 nm / min, and 39 nm / min, resulting in lower deposition efficiency. The arc counts were also high, at 12 / h, 18 / h, and 9 / h, respectively, leading to frequent arcing that severely impacted sputtering stability and film quality. Additionally, the film thickness uniformity was only ±8.5%, ±12.3%, and ±7.4%, indicating poor film thickness consistency and making it difficult to meet the requirements for high-precision coating.

[0062] In summary, since the target materials prepared in Examples 1-3 have higher density and better conductivity, the current distribution is more uniform and the plasma excitation is more stable during sputtering, effectively suppressing the generation of electric arcs. At the same time, the sputtering rate and the uniformity of film deposition are improved, thereby significantly improving the coating quality and production efficiency.

[0063] Furthermore, this invention also verified the thermal cycling stability of the Mo-ZrN biphase composite targets prepared in Examples 1-3 and Comparative Examples 1-3. As can be seen from Table 1, after 100 thermal cycles, the interface states of Examples 1-3 were no cracks, no change, and no cracks, respectively, showing excellent thermal stability; while the interfaces of Comparative Examples 1-3 showed microcracks, obvious loosening, and crack propagation, respectively, indicating severe interface failure.

[0064] In summary, the method for preparing Mo-ZrN dual-phase composite targets using hot isostatic pressing provided by this invention can significantly improve the interfacial bonding strength, electrical conductivity, sputtering stability, and film deposition uniformity of the target, and the overall performance of the target has outstanding advantages.

[0065] The above description is merely a specific embodiment of the present invention, enabling those skilled in the art to understand or implement the invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention.

[0066] It should be understood that the present invention is not limited to the content already described above, and various modifications and changes can be made without departing from its scope. The scope of the present invention is limited only by the appended claims.

Claims

1. A method for preparing Mo-ZrN dual-phase composite targets by hot isostatic pressing, characterized in that, Includes the following steps: S1. Mo powder and ZrN powder are subjected to cold isostatic pressing, sintering, first hot isostatic pressing and first annealing respectively to obtain Mo target blank and ZrN target blank. S2. The Mo target blank and ZrN target blank are pretreated respectively, and then a transition layer is filled between them to obtain a composite blank. The composite blank is placed in a sleeve, and then subjected to staged heating, sealing and welding and a second hot isostatic pressing to obtain a Mo-ZrN dual-phase composite target blank. The Mo-ZrN dual-phase composite target blank is post-treated to finally obtain the Mo-ZrN dual-phase composite target material.

2. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S1, the particle size of both Mo powder and ZrN powder is 1~10μm, the purity is 99.90%~99.95%, and the oxygen content, nitrogen content and carbon content do not exceed 50 ppm.

3. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S1, the pressure of the cold isostatic pressing is 200~400 MPa, and the holding time is 5~15 min; the temperature of the sintering process is 1500~2000℃, and the time is 2~4 h; the pressure of the first hot isostatic pressing is 150~200 MPa, the holding time is 2~5 h, and the temperature is 1500~1800°C; the holding temperature of the first annealing is 1000~1400℃, and the holding time is 1~4 h.

4. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S2, the pretreatment includes grinding, polishing and cleaning in sequence; after pretreatment, the surface roughness of the Mo target blank and the ZrN target blank is ≤0.8μm and the flatness is <0.05 mm.

5. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S2, the staged heating includes a low-temperature heating stage and a high-temperature heating stage. The temperature of the low-temperature heating stage is 200~230°C, and the holding time is 2~5h. The temperature of the high-temperature heating stage is 380~430°C, and the holding time is 2~5h. The temperature of the second hot isostatic pressing is 1200~1400°C, the pressure is 20~50MPa, and the holding time is 2~5h.

6. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S1, the thickness ratio of the Mo target blank to the ZrN target blank is 1:

1.

7. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S2, the transition layer is made of Ti and TiN dual-phase materials, with the thickness of Ti material being 5~20 µm and the thickness of TiN material being 5~10 µm.

8. The method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to claim 1, characterized in that, In S2, the post-processing operation includes a second annealing, cutting, and polishing in sequence; the holding temperature of the second annealing is 1000~1100℃, and the holding time is 1~2h; after polishing, the surface roughness Ra of the Mo-ZrN dual-phase composite target is <0.5μm.

9. A method for preparing Mo-ZrN dual-phase composite target material by hot isostatic pressing according to any one of claims 1 to 8, for use in wear-resistant coatings, decorative coatings, and protective layers for electronic devices.

Images