Low-oxygen high-density fine-grain ruthenium target material and preparation method thereof
Spherical ruthenium powder was prepared by high-vacuum electron beam melting and plasma rotating electrode atomization, and then deoxidized and hot-pressed under a hydrogen atmosphere. This solved the problems of low oxygen, high density and fine grains of ruthenium targets in the prior art, improved the coating quality and uniformity, reduced abnormal arc discharge and microparticle generation, and improved chip yield.
Patent Information
- Application Number
- CN202510817964.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-18
- Publication Date
- 2025-10-28
AI Technical Summary
Existing technologies make it difficult to prepare ruthenium targets with low oxygen, high density, and fine grains, leading to abnormal arc discharge and excessive microparticles during the coating process, resulting in high film resistance and difficulty in achieving uniformity and high yield of nanoscale deposited films.
Ruthenium rod blanks were prepared by high-vacuum electron beam melting, and spherical ruthenium powder was prepared by plasma rotating electrode atomization. The powder was then deoxidized and hot-pressed under a hydrogen atmosphere. The oxygen content was reduced and the density was increased by high-vacuum and reducing atmosphere treatment, and the grain size was controlled.
The ruthenium target material achieved an oxygen content of ≤16ppm, a grain size of <10μm, and a density of ≥99.5%, which improved the coating quality and uniformity, reduced abnormal arc discharge and microparticle generation, and improved chip yield.
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Figure CN120843871A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of target material preparation technology, specifically to a low-oxygen, high-density, fine-grained ruthenium target and its preparation method. Background Technology
[0002] Ruthenium thin films fabricated via magnetron sputtering on ruthenium targets possess advantages such as high-temperature resistance and low resistivity at the nanoscale, making them a core metal interconnect layer for advanced integrated circuit chips in processes like magnetic storage and resistive switching memory. The prepared ruthenium films are typically several nanometers to tens of nanometers thick, placing extremely stringent requirements on the ruthenium target material: first, the target material needs high purity and low oxygen content to achieve good conductivity in the film; second, the target material's micrograins need to be small and uniform, down to several micrometers, to achieve uniform thickness of the deposited film at the nanoscale; and third, the target material needs high density, exceeding 99%, to reduce abnormal arc discharge and the number of microparticles generated during deposition, thereby improving chip yield.
[0003] Because ruthenium has a high melting point of 2334℃, current ruthenium targets are mainly formed using powder metallurgy sintering or high-temperature melting and one-time casting. Powder metallurgy sintering typically uses ruthenium powder prepared by hydrometallurgy as raw material, sintering the powder through hot pressing, hot isostatic pressing, etc. Although the resulting large-size ruthenium targets have fine grains, the irregular agglomeration of ruthenium powder results in a large specific surface area and an oxygen content typically reaching hundreds to thousands of ppm. The oxygen element in the powder usually exists on the powder surface in a stable ruthenium oxide form, making it difficult to achieve a target compaction density of 99% after sintering. The oxygen content of the target material remains as high as hundreds of ppm, which easily leads to abnormal arc discharge and excessive microparticles during the target coating process, resulting in high thin film resistivity. High-purity, low-oxygen, and high-density ruthenium targets can be prepared by one-time casting through high-frequency induction melting or high-temperature melting such as electron beam. However, due to the hardness and brittleness of ruthenium, it is difficult to perform thermomechanical deformation on the ingot to refine the grains. Therefore, the grains of the target blank formed by one-time casting are coarse, ranging from hundreds of micrometers to millimeters, which is not conducive to the uniformity of the target coating. In addition, due to thermal stress issues, it is difficult to form large-sized target blanks by one-time casting, and they are prone to deformation and breakage. Summary of the Invention
[0004] To address the problem in the prior art that it is difficult to prepare target materials with low oxygen, high density, and fine grains, the present invention provides a low oxygen, high density, fine-grained ruthenium target material and its preparation method.
[0005] To achieve the above objectives, the technical solution of the present invention is as follows:
[0006] A method for preparing a low-oxygen, high-density, fine-grained ruthenium target includes the following steps:
[0007] S1. Green blank forming: Ruthenium powder is molded or cold isostatically pressed at a pressure of 250-350MPa and a holding time of 10-15min to obtain a green blank.
[0008] S2, Electron Beam Melting: The shaped blank obtained in S1 is subjected to high-vacuum electron beam melting to obtain a low-oxygen ruthenium rod blank;
[0009] S3. Bar blank processing: The ruthenium bar blank obtained in S2 is processed into a rotating electrode bar with a diameter of 50-80mm using a CNC lathe. The surface roughness of the rotating electrode bar is Ra≤0.8μm.
[0010] S4. Plasma rotating electrode atomization powder preparation: The rotating electrode rod material obtained in S3 is used to prepare spherical ruthenium powder by plasma rotating electrode atomization.
[0011] S5. Hydrogen Atmosphere Deoxidation and Hot Press Sintering: The spherical ruthenium powder obtained in S4 is sieved, and spherical ruthenium powder with a particle size of 95-105μm is selected and filled into the hot pressing mold; firstly, hydrogen reduction deep deoxidation is carried out at 1000-1300℃ for 2-4 hours, and the hydrogen pressure is 5-7×10 4 Pa; then, sintering under hydrogen atmosphere pressure was carried out at 1300-1600℃, with a hot pressing pressure of 20-25 MPa and a hydrogen pressure of 2-3 × 10⁻⁶ Pa. 3 Sintering was carried out for 1-2 hours under conditions of Pa, followed by increasing the hot pressing pressure to 40-50 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶ MPa. -3 Continue sintering at Pa for 1-2 hours to obtain a high-density ruthenium target blank;
[0012] S6. Finished product processing: The high-density ruthenium target blank obtained in S5 is welded to the back plate and then machined using a finished product machine to finally obtain a low-oxygen, high-density, fine-grained ruthenium target material.
[0013] Furthermore, in S1, the ruthenium powder has a purity of 5N, a particle size of 1-5μm, and an oxygen content of less than 500ppm; the density of the molded preform is greater than 60%.
[0014] Furthermore, in S2, the vacuum level of the high-vacuum electron beam melting is less than 6.7 × 10⁻⁶. -4 Pa; the oxygen content of the low-oxygen ruthenium rod blank is less than 10 ppm.
[0015] Furthermore, in S4, the rotational speed of the electrode rod is 15000-18000 r / min, the atomizing cooling medium is hydrogen, the hydrogen purity is 6N, and the hydrogen pressure is 0.6-1.0 MPa.
[0016] Furthermore, in S5, the spherical ruthenium powder sieving is carried out in an argon atmosphere with a purity of 6N; the hydrogen has a purity of 6N.
[0017] This invention also includes the following technical solutions:
[0018] A low-oxygen, high-density, fine-grained ruthenium target material prepared by the above-mentioned method for preparing low-oxygen, high-density, fine-grained ruthenium target material.
[0019] Furthermore, the ruthenium target has an oxygen content ≤16ppm, a grain size <10μm, and a density ≥99.5%.
[0020] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0021] This invention provides a method for preparing a low-oxygen, high-density, fine-grained ruthenium target. First, ruthenium powder blanks are melted into ruthenium rod blanks using high-vacuum electron beam melting, reducing the oxygen content of the rod blanks to below 10 ppm. Then, spherical ruthenium powder is prepared by plasma electrode atomization, and sieving yields spherical ruthenium powder with a particle size of 95-105 μm. The spherical ruthenium powder is then deoxidized in a hydrogen atmosphere and hot-pressed in a hot-press furnace, further isolating and reducing oxygen levels. The powder preparation, sieving, and sintering processes of this invention are all carried out in a reducing atmosphere such as high vacuum, argon, and hydrogen, without contact with the atmosphere or oxygen. This fundamentally reduces or eliminates the external introduction of oxygen impurities and deeply reduces and deoxidizes the residual oxygen in the powder itself, ultimately resulting in a ruthenium target material with an oxygen content ≤16 ppm. In the plasma rotating electrode atomization powder preparation process, this invention uses hydrogen instead of conventional argon as the atomization cooling medium. Utilizing the high thermal conductivity of hydrogen, the high-temperature ruthenium melt is rapidly condensed into solid spherical powder, resulting in fine-grained spherical powder. During the hydrogen atmosphere deoxidation and hot-pressing sintering process in the hot-press furnace, hydrogen reduction treatment and hydrogen atmosphere sintering ensure that the spherical powder surface is free of an oxide layer, which is beneficial for rapid diffusion and densification between powder particles. The sintering temperature is reduced to 1°C, far below the melting point of ruthenium. The temperature range of 300℃ to 1600℃ ensures densification of the ruthenium target blank while reducing the grain growth rate. A hot-pressing pressure of 20-25 MPa is used to sinter the blank density to over 90%. Hydrogen is then removed, followed by a hot-pressing pressure of 40-50 MPa under high vacuum to continue sintering. This avoids the formation of closed micropores between powder particles, ultimately achieving both fine grains and high density in the ruthenium target material, with a grain size less than 10 μm and a relative density greater than 99.5%. Attached Figure Description
[0022] The embodiments of the present invention will be further described below with reference to the accompanying drawings, wherein:
[0023] Figure 1 A process flow diagram of the preparation method of low-oxygen, high-density, fine-grained ruthenium target material is shown;
[0024] Figure 2 SEM images of agglomerated ruthenium powder prepared by conventional hydrometallurgy are shown.
[0025] Figure 3 SEM images of spherical ruthenium powder prepared by rotating electrode atomization method are shown.
[0026] Figure 4 A schematic diagram of the microstructure of a ruthenium target is shown. Detailed Implementation
[0027] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0028] Example 1
[0029] A method for preparing a low-oxygen, high-density, fine-grained ruthenium target includes the following steps:
[0030] S1. Green blank forming: Ruthenium powder with a purity of 5N, a particle size of 1μm, and an oxygen content of less than 500ppm is molded or cold isostatically pressed at a pressure of 250MPa and a holding time of 15min to obtain a green blank with a density greater than 60%.
[0031] S2, Electron Beam Melting: The shaped blank obtained in S1 is subjected to high-vacuum electron beam melting. The vacuum degree of high-vacuum electron beam melting is less than 6.7 × 10⁻⁶. -4 Pa yields a low-oxygen ruthenium rod blank with an oxygen content of less than 10 ppm.
[0032] S3. Bar blank processing: The ruthenium bar blank obtained in S2 is processed into a rotating electrode bar with a diameter of 50mm using a CNC lathe. The surface roughness of the rotating electrode bar is Ra≤0.8μm.
[0033] S4. Plasma rotating electrode atomization powder preparation: The rotating electrode rod obtained in S3 is used to prepare spherical ruthenium powder by plasma rotating electrode atomization. The rotation speed of the electrode rod is 15000 r / min, the atomization cooling medium is hydrogen, the hydrogen purity is 6N, and the hydrogen pressure is 0.6 MPa.
[0034] S5. Hydrogen Atmosphere Deoxidation and Hot Press Sintering: The spherical ruthenium powder obtained in S4 is sieved, and spherical ruthenium powder with a particle size of 95-105μm is selected and filled into the hot pressing mold; firstly, hydrogen reduction deep deoxidation is carried out at 1000℃ for 4 hours, and the hydrogen pressure is 5×10⁻⁶. 4 Pa; then, sintering was carried out at 1300℃ under hydrogen atmosphere pressure of 20 MPa and hydrogen pressure of 2 × 10⁻⁶ Pa. 3 Sintering was carried out for 2 hours under conditions of Pa, followed by increasing the hot pressing pressure to 50 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. -3Sintering was continued at Pa for 1 hour to obtain a high-density ruthenium target blank;
[0035] S6. Finished product processing: The high-density ruthenium target blank obtained in S5 is welded to the back plate and then machined using a finished product machine to finally obtain a low-oxygen, high-density, fine-grained ruthenium target material.
[0036] Example 2
[0037] A method for preparing a low-oxygen, high-density, fine-grained ruthenium target includes the following steps:
[0038] S1. Green blank forming: Ruthenium powder with a purity of 5N, a particle size of 5μm, and an oxygen content of less than 500ppm is molded or cold isostatically pressed at a pressure of 350MPa and a holding time of 10min to obtain a green blank with a density greater than 60%.
[0039] S2, Electron Beam Melting: The shaped blank obtained in S1 is subjected to high-vacuum electron beam melting. The vacuum degree of high-vacuum electron beam melting is less than 6.7 × 10⁻⁶. -4 Pa yields a low-oxygen ruthenium rod blank with an oxygen content of less than 10 ppm.
[0040] S3. Bar blank processing: The ruthenium bar blank obtained in S2 is processed into a rotating electrode bar with a diameter of 80mm using a CNC lathe. The surface roughness of the rotating electrode bar is Ra≤0.8μm.
[0041] S4. Plasma rotating electrode atomization powder preparation: The rotating electrode rod obtained in S3 is used to prepare spherical ruthenium powder by plasma rotating electrode atomization. The rotation speed of the electrode rod is 18000 r / min, the atomization cooling medium is hydrogen, the hydrogen purity is 6N, and the hydrogen pressure is 1.0 MPa.
[0042] S5. Hydrogen Atmosphere Deoxidation and Hot Press Sintering: The spherical ruthenium powder obtained in S4 is sieved, and spherical ruthenium powder with a particle size of 95-105μm is selected and filled into the hot pressing mold; firstly, hydrogen reduction deep deoxidation is carried out at 1300℃ for 2 hours, and the hydrogen pressure is 5×10⁻⁶. 4 Pa; then, sintering was carried out at 1600℃ under hydrogen atmosphere pressure of 25 MPa and hydrogen pressure of 2-3 × 10⁻³ Pa. 3 Sintering was performed for 1 hour under conditions of Pa, followed by increasing the hot pressing pressure to 40 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. - 3 Sintering was continued at Pa for 2 hours to obtain a high-density ruthenium target blank;
[0043] S6. Finished product processing: The high-density ruthenium target blank obtained in S5 is welded to the back plate and then machined using a finished product machine to finally obtain a low-oxygen, high-density, fine-grained ruthenium target material.
[0044] Example 3
[0045] A method for preparing a low-oxygen, high-density, fine-grained ruthenium target includes the following steps:
[0046] S1. Green blank forming: Ruthenium powder with a purity of 5N, a particle size of 3μm, and an oxygen content of less than 500ppm is molded or cold isostatically pressed at a pressure of 300MPa and a holding time of 12min to obtain a green blank with a density greater than 60%.
[0047] S2, Electron Beam Melting: The shaped blank obtained in S1 is subjected to high-vacuum electron beam melting. The vacuum degree of high-vacuum electron beam melting is less than 6.7 × 10⁻⁶. -4 Pa yields a low-oxygen ruthenium rod blank with an oxygen content of less than 10 ppm.
[0048] S3. Bar blank processing: The ruthenium bar blank obtained in S2 is processed into a rotating electrode bar with a diameter of 70mm using a CNC lathe. The surface roughness of the rotating electrode bar is Ra≤0.8μm.
[0049] S4. Plasma rotating electrode atomization powder preparation: The rotating electrode rod obtained in S3 is used to prepare spherical ruthenium powder by plasma rotating electrode atomization. The rotation speed of the electrode rod is 17000 r / min, the atomization cooling medium is hydrogen, the hydrogen purity is 6N, and the hydrogen pressure is 0.8 MPa.
[0050] S5. Hydrogen Atmosphere Deoxidation and Hot Press Sintering: The spherical ruthenium powder obtained in S4 is sieved, and spherical ruthenium powder with a particle size of 95-105μm is selected and filled into the hot pressing mold; firstly, hydrogen reduction deep deoxidation is carried out at 1200℃ for 3 hours, and the hydrogen pressure is 6×10⁻⁶. 4 Pa; then, pressure sintering was carried out at 1400℃ under a hydrogen atmosphere, with a hot pressing pressure of 22 MPa and a hydrogen pressure of 2.5 × 10⁻⁶ Pa. 3 Sintering was carried out for 1.5 hours under conditions of Pa, followed by increasing the hot pressing pressure to 45 MPa, evacuating the hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. -3 Sintering was continued at Pa for 1.5 h to obtain a high-density ruthenium target blank;
[0051] S6. Finished product processing: The high-density ruthenium target blank obtained in S5 is welded to the back plate and then machined using a finished product machine to finally obtain a low-oxygen, high-density, fine-grained ruthenium target material.
[0052] Example 4
[0053] The difference between this embodiment and Embodiment 1 is that the rotational speed of the electrode rod is 16000 r / min, the deep deoxidation time is 3 h, and the hydrogen pressure is 6.5 × 10⁻⁶. 4Pa; Sintering under hydrogen atmosphere pressure was carried out at 1450℃, with a hot pressing pressure of 22 MPa and a hydrogen pressure of 2.5 × 10⁻⁶ Pa. 3 Sintering was performed for 1 hour under conditions of Pa, followed by increasing the hot pressing pressure to 40 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. -3 Sintering was continued at Pa for 2 hours to obtain a high-density ruthenium target blank.
[0054] Example 5
[0055] The difference between this embodiment and Embodiment 1 is that the rotational speed of the electrode rod is 17000 r / min, the deep deoxidation time is 2 h, and the hydrogen pressure is 7 × 10⁻⁶. 4 Pa; Sintering under hydrogen atmosphere pressure at 1500℃, with a hot pressing pressure of 24 MPa and a hydrogen pressure of 3 × 10⁻⁶. 3 Sintering was performed for 1 hour under conditions of Pa, followed by increasing the hot pressing pressure to 50 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. -3 Sintering was continued at Pa for 1.5 hours to obtain a high-density ruthenium target blank.
[0056] Example 6
[0057] The difference between this embodiment and Embodiment 1 is that the rotational speed of the electrode rod is 18000 r / min, the deep deoxidation time is 3 h, and the hydrogen pressure is 7.5 × 10⁻⁶. 4 Pa; sintering under hydrogen atmosphere pressure was carried out at 1550℃, with a hot pressing pressure of 25 MPa and a hydrogen pressure of 3 × 10⁻⁶ Pa. 3 Sintering was performed for 1 hour under conditions of Pa, followed by increasing the hot pressing pressure to 42 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶. -3 Sintering was continued at Pa for 2 hours to obtain a high-density ruthenium target blank.
[0058] Comparative Example 1
[0059] The difference between this comparative example and Example 1 is that the finished product is processed directly after electron beam melting, without the S3-S5 treatment, while other process parameters remain unchanged.
[0060] Comparative Example 2
[0061] The difference between this comparative example and Example 1 is that the ruthenium powder is only processed in S5-S6, while other process parameters remain unchanged.
[0062] The performance results of the ruthenium targets prepared in the examples and comparative examples are shown in Table 1.
[0063] Table 1
[0064]
[0065] As shown in Table 1, the ruthenium target prepared by this invention has the advantages of low oxygen, high density and fine grains, which is beneficial to the uniformity of the target coating composition and thickness.
[0066] This invention provides a method for preparing a low-oxygen, high-density, fine-grained ruthenium target. First, ruthenium powder blanks are melted into ruthenium rod blanks using high-vacuum electron beam melting, reducing the oxygen content of the rod blanks to below 10 ppm. Then, spherical ruthenium powder is prepared by plasma electrode atomization, and sieving yields spherical ruthenium powder with a particle size of 95-105 μm. The spherical ruthenium powder is then deoxidized in a hydrogen atmosphere and hot-pressed in a hot-press furnace, further isolating and reducing oxygen levels. The powder preparation, sieving, and sintering processes of this invention are all carried out in a reducing atmosphere such as high vacuum, argon, and hydrogen, without contact with the atmosphere or oxygen. This fundamentally reduces or eliminates the external introduction of oxygen impurities and deeply reduces and deoxidizes the residual oxygen in the powder itself, ultimately resulting in a ruthenium target material with an oxygen content ≤16 ppm. In the plasma rotating electrode atomization powder preparation process, this invention uses hydrogen instead of conventional argon as the atomization cooling medium. Utilizing the high thermal conductivity of hydrogen, the high-temperature ruthenium melt is rapidly condensed into solid spherical powder, resulting in fine-grained spherical powder. During the hydrogen atmosphere deoxidation and hot-pressing sintering process in the hot-press furnace, hydrogen reduction treatment and hydrogen atmosphere sintering ensure that the spherical powder surface is free of an oxide layer, which is beneficial for rapid diffusion and densification between powder particles. The sintering temperature is reduced to 1°C, far below the melting point of ruthenium. The temperature range of 300℃ to 1600℃ ensures densification of the ruthenium target blank while reducing the grain growth rate. A hot-pressing pressure of 20-25 MPa is used to sinter the blank density to over 90%. Hydrogen is then removed, followed by a hot-pressing pressure of 40-50 MPa under high vacuum to continue sintering. This avoids the formation of closed micropores between powder particles, ultimately achieving both fine grains and high density in the ruthenium target material, with a grain size less than 10 μm and a relative density greater than 99.5%.
[0067] The foregoing descriptions have outlined some exemplary embodiments of the present invention. It is understood that these embodiments are merely illustrative and do not constitute a limitation on the scope of protection of the present invention. Features in these embodiments can be rearranged in suitable ways, and the resulting solutions remain within the scope of protection claimed by the present invention. All other embodiments obtained by those skilled in the art based on the foregoing embodiments without inventive effort, i.e., all modifications, equivalent substitutions, and improvements made within the spirit and principles of this application, fall within the scope of protection claimed by the present invention.
Claims
1. A method for preparing a low-oxygen, high-density, fine-grained ruthenium target, characterized in that, Includes the following steps: S1. Green blank forming: Ruthenium powder is molded or cold isostatically pressed at a pressure of 250-350MPa and a holding time of 10-15min to obtain a green blank. S2, Electron Beam Melting: The shaped blank obtained in S1 is subjected to high-vacuum electron beam melting to obtain a low-oxygen ruthenium rod blank; S3. Bar blank processing: The ruthenium bar blank obtained in S2 is processed into a rotating electrode bar with a diameter of 50-80mm using a CNC lathe. The surface roughness of the rotating electrode bar is Ra≤0.8μm. S4. Plasma rotating electrode atomization powder preparation: The rotating electrode rod material obtained in S3 is used to prepare spherical ruthenium powder by plasma rotating electrode atomization. S5. Hydrogen Atmosphere Deoxidation and Hot Press Sintering: The spherical ruthenium powder obtained in S4 is sieved, and spherical ruthenium powder with a particle size of 95-105μm is selected and filled into the hot pressing mold; firstly, hydrogen reduction deep deoxidation is carried out at 1000-1300℃ for 2-4 hours, and the hydrogen pressure is 5-7×10 4 Pa; then, sintering under hydrogen atmosphere pressure was carried out at 1300-1600℃, with a hot pressing pressure of 20-25 MPa and a hydrogen pressure of 2-3 × 10⁻⁶ Pa. 3 Sintering was carried out for 1-2 hours under conditions of Pa, followed by increasing the hot pressing pressure to 40-50 MPa, removing hydrogen gas, and maintaining a vacuum degree of less than 6.7 × 10⁻⁶ MPa. -3 Continue sintering at Pa for 1-2 hours to obtain a high-density ruthenium target blank; S6. Finished product processing: The high-density ruthenium target blank obtained in S5 is welded to the back plate and then machined using a finished product machine to finally obtain a low-oxygen, high-density, fine-grained ruthenium target material.
2. The method for preparing a low-oxygen, high-density, fine-grained ruthenium target according to claim 1, characterized in that, In S1, the ruthenium powder has a purity of 5N, a particle size of 1-5μm, and an oxygen content of less than 500ppm; the density of the molded preform is greater than 60%.
3. The method for preparing a low-oxygen, high-density, fine-grained ruthenium target according to claim 1, characterized in that, In S2, the vacuum level of high-vacuum electron beam melting is less than 6.7 × 10⁻⁶. -4 Pa; the oxygen content of the low-oxygen ruthenium rod blank is less than 10 ppm.
4. The method for preparing a low-oxygen, high-density, fine-grained ruthenium target according to claim 1, characterized in that, In S4, the rotational speed of the electrode rod is 15000-18000 r / min, the atomizing cooling medium is hydrogen, the hydrogen purity is 6N, and the hydrogen pressure is 0.6-1.0 MPa.
5. The method for preparing a low-oxygen, high-density, fine-grained ruthenium target according to claim 1, characterized in that, In S5, spherical ruthenium powder sieving is carried out in an argon atmosphere with a purity of 6N; hydrogen has a purity of 6N.
6. A low-oxygen, high-density, fine-grained ruthenium target prepared by the preparation method of the low-oxygen, high-density, fine-grained ruthenium target according to any one of claims 1-5.
7. The low-oxygen, high-density, fine-grained ruthenium target material according to claim 6, characterized in that, The ruthenium target has an oxygen content of ≤16ppm, a grain size of <10μm, and a density of ≥99.5%.