WO2021046928A1 - Matériau cible rotatif de ni-v de grand diamètre de tube contenant des éléments traces et son procédé de préparation - Google Patents

Matériau cible rotatif de ni-v de grand diamètre de tube contenant des éléments traces et son procédé de préparation Download PDF

Info

Publication number
WO2021046928A1
WO2021046928A1 PCT/CN2019/108213 CN2019108213W WO2021046928A1 WO 2021046928 A1 WO2021046928 A1 WO 2021046928A1 CN 2019108213 W CN2019108213 W CN 2019108213W WO 2021046928 A1 WO2021046928 A1 WO 2021046928A1
Authority
WO
WIPO (PCT)
Prior art keywords
diameter
trace elements
rotating target
containing trace
temperature
Prior art date
Application number
PCT/CN2019/108213
Other languages
English (en)
Chinese (zh)
Inventor
吴宇宁
卿海标
周其刚
Original Assignee
南京达迈科技实业有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 南京达迈科技实业有限公司 filed Critical 南京达迈科技实业有限公司
Publication of WO2021046928A1 publication Critical patent/WO2021046928A1/fr

Links

Images

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/02—Making non-ferrous alloys by melting
    • C22C1/023—Alloys based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/03—Alloys based on nickel or cobalt based on nickel
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/10—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of nickel or cobalt or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering

Definitions

  • the invention relates to a magnetron sputtering target material and its preparation, in particular to a large-diameter Ni-V rotating target material containing trace elements and a preparation method thereof.
  • Magnetron sputtering coating technology which occupies an important position in the coating field, is also being further improved.
  • Target materials are the most critical basic consumables in the magnetron sputtering coating process. Only the most suitable target materials with high utilization rate, high quality and high quality can fully meet the demand and drive the development of science and technology.
  • the magnetron sputtering coating technology of nickel-vanadium targets has a relatively large market in the domestic solar field, but most of the nickel-vanadium targets are flat targets, and rotating targets only account for a small part.
  • the main reason is that the current domestic technology can only mass-produce some small-diameter nickel-vanadium rotating targets with a diameter of less than 100mm.
  • Large-diameter nickel-vanadium rotating targets with a diameter of more than 100mm are produced in the traditional pipe-piercing and rolling process. It requires multiple reaming and mold replacement, and the cost is quite high, and defects such as cracks, inclusions and eccentricity often occur, the scrap rate is extremely high, and the cost is too high.
  • the utilization rate of the rotating target can be as high as 70%, especially the utilization rate of the large-diameter nickel-vanadium rotating target can be as high as 80% and above, and the utilization rate of the large-diameter nickel-vanadium rotating target can be as high as 80% and above.
  • the nickel-vanadium rotating target can also be bound by brazing material to meet more market demands. Therefore, it is imperative to find a method for preparing a large-diameter nickel-vanadium rotating target with suitable composition, simple production process, high yield, high precision, and low cost.
  • One of the objectives of the present invention is to provide a large-diameter Ni-V rotating target containing trace elements, which uses the addition of trace elements C, B, Ti, and Mg to improve the performance of the rotating target;
  • the second purpose is to provide a method for preparing a large-diameter Ni-V rotating target containing trace elements, which can overcome the problems of nickel-vanadium tube cracking, inclusions, defects, eccentricity, and processing difficulties. Vanadium rotating target.
  • the large-diameter Ni-V rotating target containing trace elements of the present invention includes the following raw material components in terms of mass percentage: C 0.01-0.05%, B 0.01-0.08%, Ti 0.001-0.006%, Mg 0.01 ⁇ 0.05%, V 6 ⁇ 8%, the balance Ni and unavoidable impurities. Among them, the inevitable impurities such as Al, Fe and so on.
  • the present invention also provides a method for preparing the large-diameter Ni-V rotating target material containing trace elements.
  • the preparation steps mainly include raw material preparation, vacuum melting, hot forging, machining, hot extrusion, pickling treatment, Solution treatment, cold rolling or boring, annealing treatment, machining or binding; the specific process is:
  • Vacuum smelting prepare raw materials before smelting, graphite with purity ⁇ 99.9, boron particles with purity ⁇ 99.9, metallic titanium with purity ⁇ 99.9, metallic magnesium with purity ⁇ 99.9, metallic vanadium with purity ⁇ 99.9, electrolytic nickel with purity ⁇ 99.96; Then, the raw materials are mixed with electrolytic nickel, metallic vanadium, and graphite according to the content of the above-mentioned components, and then smelted in a vacuum at 1400-1550°C for 70-90 minutes, and then titanium, magnesium, and boron are added for refining for 10-20 minutes, and then under a protective atmosphere The ingot is obtained by casting; wherein the vacuum degree is kept at less than 4 Pa during the whole smelting process; the protective atmosphere during casting can be argon;
  • Hot forging rough machining of the ingot before hot forging.
  • the lathe can be used to remove the surface oxide scale and some defects, and the riser can be cut to obtain a round truncated cone-shaped bright ingot, which is carefully ground to remove microcracks, etc.;
  • the ingot is hot forged, the ingot is heated to 1090 ⁇ 1120°C, and after holding for 20 ⁇ 50min, forging is carried out, the forging temperature is 1090 ⁇ 1120°C, and the final forging temperature is 990 ⁇ 1050°C; the ingot is repeatedly roughed and then drawn Long, the deformation is greater than 50%; the deformation of the drawing here is greater than 50%, which is compared with the forging rod after the pier is thick.
  • Hot extrusion The alloy cylinder obtained in step (3) is heated by induction heating at a heating temperature of 990 to 1130°C; then the hole is expanded at a speed of 150 to 220 mm/s; and then a secondary induction is used Heat treatment, the heating temperature is 1000 ⁇ 1150°C, and the hot extruder is used for extrusion, and the extrusion speed is 120 ⁇ 150mm/s;
  • Pickling treatment the waste pipe is pickled to remove defects such as surface pits; the pickling treatment can adopt the common pickling process in the prior art.
  • Solution treatment The acid-washed waste pipe is solid-solution treated to obtain a single-phase austenite structure at room temperature, so that the material has the best corrosion resistance, high plasticity, good formability, and can refine the waste pipe The grain structure.
  • the surface-treated waste tube is rolled or bored with high precision to obtain a bright tube with an inner hole size tolerance of ⁇ 0.2mm.
  • Annealing treatment the bright tube is annealed, the annealing temperature is 840 ⁇ 870°C, and the heat preservation is 80 ⁇ 90min.
  • the bright tube is processed to the overall rotating target of the required size, or processed to a certain size, and then the binding rotating target of the required size is made by binding.
  • the electrolytic nickel is baked at 580-620° C. for 5-8 hours. Long-term baking can effectively remove most of the hydrogen contained in electrolytic nickel.
  • titanium, magnesium, and boron are added in the vacuum melting process by using nickel foil to enclose the titanium, magnesium, and boron; during the vacuum melting process, the micro-alloying elements metal titanium and metal magnesium are added in the above-mentioned manner.
  • Boron particles can avoid boiling and sputtering of molten steel caused by direct addition.
  • the deformation of the pier thickness in the step (2) is greater than 50%.
  • the pier roughening and drawing length are repeated, the pier rough deformation is more than 50%, and the coarse grain structure is fully broken, thereby increasing the extrusion yield.
  • the diameter of the central through hole in the step (3) is 20-40 mm, and the taper of the tapered hole is 20°-40°.
  • the central through hole and tapered hole here facilitate the reaming head to correspond to the alloy, and prevent eccentricity caused by reaming.
  • the temperature of the secondary induction heating is 10-20°C higher than the temperature of the previous induction heating. Enlarging the hole after induction heating, and then extruding after the second induction heating; and the temperature of the second induction heating is slightly higher by 10-20°C, which can prevent defects or scrapping in the extrusion process caused by the temperature drop during the extrusion preparation process .
  • the waste pipe is heated to 950-1000° C. for heat preservation, and then water quenched.
  • a solution treatment at a lower temperature and rapid cooling are adopted to obtain a waste tube with fine grains and improve the plasticity and corrosion resistance of the material.
  • annealing treatment annealing the bright tube, the annealing temperature is 840-870°C, and the heat preservation is 80-90 min.
  • the present invention optimizes the composition by adding trace elements C, B, Ti, Mg in the high vacuum smelting process, reduces the content of oxygen, sulfur, etc., and can inhibit the initiation of cracks, and improve the grain boundary bonding force of the target material. Strength, and refine the grains, thereby increasing the yield.
  • adding B element, B segregates on the grain boundary or vacancy type defects, improves the grain boundary bonding force, forms fine M 3 B 2 type borides, and reduces the formation of ⁇ phase in the TCP phase formed by the combination of impurity elements , Inhibit the generation of cracks; due to the relatively high viscosity of nickel and vanadium during the smelting process, it is difficult to feed during the solidification process.
  • element B can improve the feeding of the alloy in the later stage of solidification and reduce the generation of microscopic shrinkage; adding Ti Since the impurity element Al and Ni in the alloy form a Ni 3 Al intermetallic compound, the addition of Ti can replace the Al atom in Ni 3 Al to form a Ni 3 (Al, Ti) type strengthening phase, thereby further improving the alloy’s Strength; adding C and Mg elements, mainly for deoxidation, desulfurization, and purification of molten metal, and will volatilize at high temperatures, and does not affect the purity of molten metal. Thereby reducing the content of interstitial gases such as hydrogen, oxygen and nitrogen in the nickel-vanadium alloy, while removing harmful sulfur impurities and refining crystal grains. Thereby improving the quality of the alloy and optimizing the alloy composition.
  • interstitial gases such as hydrogen, oxygen and nitrogen in the nickel-vanadium alloy
  • the large-diameter Ni-V rotating target containing trace elements in the present invention is very critical in hot forging and hot extrusion temperature during the hot working process.
  • the nickel-based alloy Ni93V7
  • the research method of thermal processing map of dynamic material model has now become the most effective method to study the workability of metal materials and control the deformed structure.
  • a thermal simulation single-pass compression experiment was performed on a nickel-based alloy (Ni93V7).
  • three sets of rates were set, namely 0.001s -1 , 0.1s -1 , and 1s -1 , and each set of rates set four temperatures: 1000 °C, 1050°C, 1100°C, 1150°C.
  • the thermal deformation behavior of the new material is systematically explored.
  • the thermal processing diagram of the nickel-based alloy is drawn. Based on the flow stress curve of the nickel-vanadium alloy, the power dissipation of the alloy based on the dynamic material model is established Figure. Because there is no instability phenomenon, the generation of the thermal processing map does not need to superimpose the power dissipation map and the rheological instability map.
  • the power dissipation map is the final thermal processing map.
  • the best hot working parameters of nickel-vanadium alloy are in the interval of 1090 ⁇ 1120°C, 1s -1.
  • the two key technical links of the present invention are the ratio design of the Ni-V rotating target material and the control of the process conditions, which are complementary to each other.
  • Ni-V rotating targets have been successfully prepared through suitable component ratios and optimized preparation methods.
  • the entire rotating target can be made or bound with the rotating target to meet more requirements. More usage needs.
  • the present invention adds a small amount of alloying elements C, B, Ti, Mg to optimize the composition, reduces the content of oxygen, sulfur, etc., and can inhibit the initiation of cracks, and improve the grain boundary bonding of the target material Strength, strength, and grain refinement can improve the feeding of the alloy in the later stage of solidification, reduce the generation of microscopic shrinkage, and increase the yield.
  • Electrolytic nickel can effectively remove part of the hydrogen contained in electrolytic nickel through long-term high-temperature baking; through repeated thickening and elongation forging process, hole expansion after induction heating, and extrusion and finish rolling after secondary induction heating Or boring and other technological processes can improve the concentricity and yield rate of the rotating target;
  • the present invention does not need to add rare earth elements, and successfully prepares a large diameter Ni-V rotating target with low cost and excellent performance through the optimization of the composition and the control of the process conditions;
  • the present invention draws the hot processing diagram of the nickel-based alloy, obtains the hot forging and hot extrusion optimization parameters of the rotating target, and greatly improves the finished product of the large-diameter Ni-V rotating target rate;
  • the preparation method of the present invention can overcome the problems of nickel-vanadium tube cracking, inclusions, defects, eccentricity, and processing difficulties, etc., a large-diameter nickel-vanadium rotating target material;
  • the present invention can achieve 70%-80% utilization rate by manufacturing an integral rotating target or a bound rotating target, which can not only meet more market demands and special demands, but also increase the utilization rate of materials and reduce costs.
  • Figure 1 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 1;
  • Example 2 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 2;
  • Example 3 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 3;
  • Example 4 is a 100 times metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 4;
  • Example 5 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 5;
  • Fig. 6 is a 100-fold metallographic photograph of the large-diameter Ni-V rotating target prepared in Example 6;
  • Figure 7 is a low-magnification photo of the comparative example during the preparation of Ni-V rotating target
  • Figure 8 is a 100-fold metallographic picture of the target of the comparative example.
  • the reagents and materials used to prepare the large-diameter Ni-V rotating target in the following examples are all commercially available.
  • composition and content of the large-diameter Ni-V rotating target containing trace elements are as follows: C 0.02%, B 0.03%, Ti 0.005%, Mg 0.01%, V 6% and The balance Ni and unavoidable impurities.
  • the preparation method of the large diameter Ni-V rotating target includes the following steps:
  • Vacuum melting prepare raw material graphite, boron particles, metallic titanium, metallic magnesium, metallic vanadium, electrolytic nickel, among which the purity of raw materials is 99.9% graphite, 99.9% boron particles, 99.9% metallic titanium, 99.9% Metal magnesium, 99.9% metallic vanadium, 99.96% electrolytic nickel;
  • the surface oil stains and oxides of electrolytic nickel and metal vanadium are cleaned and dried and weighed. Then, the electrolytic nickel is baked at 600°C for 6 hours; then the raw materials are prepared according to the content of the above components.
  • the electrolytic nickel, metal vanadium, Graphite is put into a vacuum melting crucible and smelted with electricity. The melting temperature is 1500°C, and the melting time is 80 minutes. Then, the metal titanium, metal magnesium and boron particles wrapped in nickel foil are added successively, and then refined for 15 minutes.
  • the vacuum degree during the entire melting process Less than 4Pa; casting is performed after smelting, and argon gas 4Mpa is passed in a vacuum state before casting, and the casting is performed under protective atmosphere conditions, and the ingot is demolded after 40 minutes of casting.
  • the first machining Use a lathe to remove the oxide scale and some defects on the surface of the ingot, cut off the riser to obtain a round truncated cone-shaped bright ingot, and carefully grind to remove microcracks, etc.;
  • Hot forging heat the machined ingot to 1100°C, hold for 30 minutes, and then perform forging.
  • the forging temperature is 1100°C and the final forging temperature is 1000°C; the ingot is repeatedly thickened and thickened.
  • the amount of deformation is 60%, and then the drawing is carried out, and the drawing deformation is 60%; the drawing deformation here is compared with the forging rod after the pier is thick; the final forging is Forging rod
  • Second machining remove the oxide scale on the surface of the cylindrical forging rod, and process both ends of the forging rod to be flat, ensuring that the end face is perpendicular to the cylindrical surface, and after machining, it will be a cylinder with a diameter of 300 ⁇ 3 mm and a length greater than 500 mm. Processed a central through hole with a diameter of 30mm, and processed a tapered hole with a 20° taper at one end to obtain an alloy cylinder;
  • Hot extrusion The alloy cylinder is heated by induction heating at a heating temperature of 1000°C, and then the hole is expanded by a reaming head at a reaming speed of 200mm/s, and then subjected to secondary induction heating at a heating temperature of 1020. °C, and then use a 6500-ton hot extruder for extrusion at a speed of 120mm/s to obtain a waste pipe with an outer diameter of 170-200mm, an inner diameter of 130-160mm, and a length of 2500-4500mm;
  • Annealing treatment under the condition of annealing temperature of 850°C, annealing holding time is 80min for annealing treatment;
  • the bright tube is processed to the overall rotating target of the required size, or processed to a certain size, and then the binding rotating target of the required size is made by binding.
  • the metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out.
  • the metallographic picture under 100 times is shown in Figure 1. It can be seen that there are fine precipitates dispersed at the grain boundary, thus Play a strengthening effect, the grain distribution is uniform, and the average grain size is 47-63 ⁇ m.
  • the composition and content of the large-diameter Ni-V rotating target are as follows: C 0.03%, B 0.01%, Ti 0.003%, Mg 0.03%, V 7% and the balance Ni and Inevitable impurities.
  • the preparation method of the large-diameter Ni-V rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (1) the electrolytic nickel is baked at 580°C for 5 hours; the melting temperature is 1450°C, the melting time is 70 minutes, and the refining time is 10 minutes;
  • step (3) the ingot is heated to 1090°C and held for 20 minutes before forging.
  • the forging temperature is 1090°C and the final forging temperature is 1000°C;
  • the deformation of the pier thickness is 55%, and the deformation after drawing is 55%;
  • step (4) a central through hole with a diameter of 20mm is machined, and one end is machined into a tapered hole with a 30° taper;
  • step (5) the induction heating temperature is 1100°C, and the hole expanding speed is 180mm/s; the second induction heating temperature is 1110°C, and the extrusion speed is 130mm/s;
  • step (7) the solution treatment is heated to 980°C;
  • step (9) the annealing temperature is 840° C., and the annealing holding time is 85 min.
  • composition and content of the large-diameter Ni-V rotating target in this embodiment are as follows in terms of mass percentage: C 0.05%, B 0.08%, Ti 0.001%, Mg 0.05%, V 8%, and the balance Ni and Inevitable impurities.
  • the preparation method of the large-diameter Ni-V rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (1) the electrolytic nickel is baked at 610°C for 8 hours; the melting temperature is 1400°C, the melting time is 90 minutes, and the refining time is 20 minutes;
  • step (3) the ingot is heated to 1110°C and kept for 40 minutes before forging.
  • the forging temperature is 1110°C and the final forging temperature is 990°C; the deformation of the upset thickness is 65%;
  • step (4) a central through hole with a diameter of 30mm is machined, and a tapered hole with a 40° taper is machined at one end;
  • step (5) the induction heating temperature is 990°C, and the hole expanding speed is 150mm/s; the second induction heating temperature is 1000°C, and the extrusion speed is 140mm/s;
  • step (7) the solution treatment is heated to 970°C;
  • step (9) the annealing temperature is 860°C, and the annealing holding time is 90 min.
  • the metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out.
  • the metallographic picture at 100 times is shown in Figure 3. It can be seen that a small amount of fine precipitates are distributed at the grain boundaries, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 45-73 ⁇ m.
  • composition and content of the large-diameter Ni-V rotating target in this embodiment are as follows in terms of mass percentage: C 0.03%, B 0.05%, Ti 0.002%, Mg 0.04%, V 6% and the balance Ni and Inevitable impurities.
  • the preparation method of the large-diameter Ni-V rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (1) the electrolytic nickel is baked at 620°C for 7 hours; the smelting temperature is 1550°C, and the smelting time is 70min;
  • step (3) the ingot is heated to 1120°C and held for 50 minutes before forging.
  • the forging temperature is 1120°C and the final forging temperature is 1050°C; the deformation of the upset thickness is 55%;
  • step (4) a central through hole with a diameter of 40mm is machined, and a tapered hole with a 40° taper is machined at one end;
  • step (5) the induction heating temperature is 1050°C, and the hole expanding speed is 200mm/s; the second induction heating temperature is 1060°C, and the extrusion speed is 150mm/s;
  • step (7) the solution treatment is heated to 1000°C;
  • step (9) the annealing temperature is 870°C, and the annealing holding time is 90 minutes.
  • the metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out.
  • the metallographic picture at 100 times is shown in Figure 4. It can be seen that there are fine precipitates dispersed at the grain boundary, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 47-80 ⁇ m.
  • composition and content of the large-diameter Ni-V rotating target are as follows in terms of mass percentage: C 0.04%, B 0.06%, Ti 0.006%, Mg 0.02%, V 7%, and the balance Ni and Inevitable impurities.
  • the preparation method of the large-diameter Ni-V rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (1) the electrolytic nickel is baked at 590°C for 6 hours;
  • step (4) a central through hole with a diameter of 20mm is machined, and a tapered hole with a 40° taper is machined at one end;
  • step (5) the induction heating temperature is 1130°C, and the reaming speed is 220mm/s; the second induction heating temperature is 1150°C, and the extrusion speed is 130mm/s;
  • step (7) the solution treatment is heated to 960°C;
  • the metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out.
  • the metallographic picture at 100 times is shown in Figure 5. It can be seen that there are fine precipitates dispersed in the grain boundary, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 40-54 ⁇ m.
  • composition and content of the large-diameter Ni-V rotating target are as follows in terms of mass percentage: C 0.01%, B 0.02%, Ti 0.002%, Mg 0.01%, V 8%, and the balance Ni and Inevitable impurities.
  • the preparation method of the large-diameter Ni-V rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (1) the electrolytic nickel is baked at 590°C for 6 hours;
  • step (4) a central through hole with a diameter of 20mm is machined, and a tapered hole with a 40° taper is machined at one end;
  • step (5) the induction heating temperature is 1120°C, and the reaming speed is 160mm/s; the second induction heating temperature is 1140°C, and the extrusion speed is 125mm/s;
  • step (7) the solution treatment is heated to 1000°C.
  • the metallographic analysis of the large-diameter Ni-V rotating target prepared in this example is carried out.
  • the metallographic picture at 100 times is shown in Figure 6. It can be seen that a small amount of fine precipitates are distributed at the grain boundaries, thus Play a strengthening effect, the grain distribution is relatively uniform, and the average grain size is 45-69 ⁇ m.
  • This comparative example is basically the same as Example 1, except that:
  • step (3) the ingot is heated to 1150°C, and after holding for 50 minutes, forging is performed, the opening forging temperature is 1150°C, and the final forging temperature is 1000°C;
  • step (5) the induction heating temperature is 1140°C; the second induction heating temperature is 1160°C.
  • the Ni-V target material of this comparative example was severely cracked after hot extrusion, and obvious cracks can be seen; from Figure 8, it can be seen that the grains are relatively coarse.
  • the grain size is between 80-100 ⁇ m, the inclusions at the grain boundary are coarse, and the grain boundary is damaged; therefore, the appropriate hot forging temperature and hot extrusion temperature are very important.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Forging (AREA)
  • Extrusion Of Metal (AREA)

Abstract

L'invention concerne un matériau cible rotatif de Ni-V de grand diamètre contenant des éléments traces et son procédé de préparation. Le matériau cible rotatif comprend les constituants suivants, en pourcentage en masse : 0,01 à 0,05 % de C, 0,01 à 0,08 % de B, 0,001 à 0,006 % de Ti, 0,01 à 0,05 % de Mg, 6 à 8 % de V, et le reste étant du Ni et des impuretés inévitables. Les étapes de préparation utilisent successivement une fusion sous vide, un forgeage à chaud, un usinage, un pressage à chaud, un traitement de décapage à l'acide, un traitement par une solution, un laminage à froid ou un alésage, un traitement de recuit, et un usinage ou une liaison. Sur la base du Ni-V, la présente invention optimise les ingrédients en ajoutant des éléments traces C, B, Ti et Mg, et diminue la teneur en oxygène, soufre, etc., et la présente invention peut inhiber la création de fissures, améliore la force de liaison de limite de grain et la résistance du matériau cible, et affine les grains cristallins, ce qui permet d'améliorer le rendement ; en outre, l'invention réduit le taux de rejet par optimisation des paramètres de traitement à chaud.
PCT/CN2019/108213 2019-09-12 2019-09-26 Matériau cible rotatif de ni-v de grand diamètre de tube contenant des éléments traces et son procédé de préparation WO2021046928A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910869200.3 2019-09-12
CN201910869200.3A CN110468382B (zh) 2019-09-12 2019-09-12 一种含微量元素的大管径Ni-V旋转靶材及其制备方法

Publications (1)

Publication Number Publication Date
WO2021046928A1 true WO2021046928A1 (fr) 2021-03-18

Family

ID=68515848

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/CN2019/108213 WO2021046928A1 (fr) 2019-09-12 2019-09-26 Matériau cible rotatif de ni-v de grand diamètre de tube contenant des éléments traces et son procédé de préparation

Country Status (2)

Country Link
CN (1) CN110468382B (fr)
WO (1) WO2021046928A1 (fr)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111004985B (zh) * 2019-11-25 2021-05-11 有研亿金新材料有限公司 一种镍钒溅射靶材的制备方法
CN111304606A (zh) * 2020-03-30 2020-06-19 宁波江丰电子材料股份有限公司 无缺陷高纯镍钒靶坯的制备方法及利用其制备得到的靶材
CN112663006A (zh) * 2020-12-18 2021-04-16 宝鸡市亨信稀有金属有限公司 一种镍钒合金管靶及生产方法
CN112845659B (zh) * 2021-01-05 2022-09-16 太原科技大学 一种uns n06600小口径精密无缝管的制备方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4552820A (en) * 1984-04-25 1985-11-12 Lin Data Corporation Disc media
JP2000313954A (ja) * 1999-03-31 2000-11-14 Praxair St Technol Inc アルファ放射が極少のニッケル／バナジウム・スパッタリング・ターゲットを製造する方法
CN1723292A (zh) * 2002-12-09 2006-01-18 霍尼韦尔国际公司 高纯镍/钒溅射构件和制备溅射构件的方法
CN1852998A (zh) * 2003-10-07 2006-10-25 株式会社日矿材料 高纯度Ni－V合金、由该Ni－V合金形成的靶以及该Ni－V合金薄膜和高纯度Ni－V合金的制造方法
CN103710577A (zh) * 2014-01-16 2014-04-09 南京达迈科技实业有限公司 含微量稀土元素的镍钒合金磁控溅射旋转靶材及制备方法
CN104014767A (zh) * 2014-06-05 2014-09-03 贵研铂业股份有限公司 一种制备NiV合金靶材的方法

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105734507B (zh) * 2016-04-05 2018-06-19 基迈克材料科技（苏州）有限公司 成膜均匀的细晶镍合金旋转靶材及其热挤压优化制备方法
CN107190158B (zh) * 2017-05-19 2019-01-11 江苏隆达超合金航材有限公司 降低镍基高温合金中o、n、s含量的真空感应熔炼工艺
CN108384992A (zh) * 2018-04-20 2018-08-10 温州市赢创新材料技术有限公司 一种高强度耐腐蚀镍基高温合金及其制造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4552820A (en) * 1984-04-25 1985-11-12 Lin Data Corporation Disc media
JP2000313954A (ja) * 1999-03-31 2000-11-14 Praxair St Technol Inc アルファ放射が極少のニッケル／バナジウム・スパッタリング・ターゲットを製造する方法
CN1723292A (zh) * 2002-12-09 2006-01-18 霍尼韦尔国际公司 高纯镍/钒溅射构件和制备溅射构件的方法
CN1852998A (zh) * 2003-10-07 2006-10-25 株式会社日矿材料 高纯度Ni－V合金、由该Ni－V合金形成的靶以及该Ni－V合金薄膜和高纯度Ni－V合金的制造方法
CN103710577A (zh) * 2014-01-16 2014-04-09 南京达迈科技实业有限公司 含微量稀土元素的镍钒合金磁控溅射旋转靶材及制备方法
CN104014767A (zh) * 2014-06-05 2014-09-03 贵研铂业股份有限公司 一种制备NiV合金靶材的方法

Also Published As

Publication number Publication date
CN110468382B (zh) 2021-04-09
CN110468382A (zh) 2019-11-19

Similar Documents

Publication Publication Date Title
WO2021046928A1 (fr) Matériau cible rotatif de ni-v de grand diamètre de tube contenant des éléments traces et son procédé de préparation
CN108823472B (zh) 一种高强韧Al-Zn-Mg-Cu系铝合金及其热处理方法
WO2021174726A1 (fr) Alliage à haute température déformé à base de nickel ayant une teneur élevée en aluminium et son procédé de préparation
CN109355530B (zh) 一种耐热钛合金丝材的制备方法和应用
CN100519813C (zh) 高强韧性冷作模具钢及其制备方法
CN112695255B (zh) 一种铁素体马氏体钢包壳管材制备方法
CN109161727B (zh) 一种电弧/电子束熔丝增材制造用钛合金及其制备方法
CN101654764B (zh) 一种铁镍基高弹性合金及其毛细管和毛细管的制造方法
CN109234554B (zh) 一种高温钛合金棒材的制备方法
CN112139415B (zh) 一种补偿加热辅助自由锻生产难变形镍基高温合金的方法
CN114645162A (zh) 一种难变形高温合金的细晶均质盘锻件的制造方法
CN108504897A (zh) 一种近β型钛合金及该钛合金棒材的锻造方法
CN104372216B (zh) 一种7a04铝合金的热顶铸造工艺及其铝合金
CN108977689B (zh) 一种亚稳β钛合金板材及其加工方法
CN111850372A (zh) 一系列FeCoCrNiW(VC)X高熵合金的制备及其沉淀强化工艺
CN114107834B (zh) 一种高强铁镍钼合金丝材及其低成本制备方法
WO2021046929A1 (fr) Cible rotative de ni-cr de grand diamètre contenant des éléments de trace et son procédé de préparation
CN106334883A (zh) 一种高强度、耐腐蚀的高温铜基钎焊料及其制造方法
CN114905188A (zh) 耐腐蚀耐高温镍基合金焊丝及其制备方法
CN111850349B (zh) 一种钴基高温合金的热加工方法
CN109778002A (zh) 一种用于丝材3d打印的稀土钛合金
CN104404325B (zh) 一种7085铝合金的热顶铸造工艺及其铝合金
CN109182906A (zh) 一种耐高温高强度螺帽及其生产方法
CN113897513B (zh) 一种1200MPa级耐硝酸腐蚀高强度钛合金及其制备方法
CN115404383B (zh) 一种核电用高强度镍基合金丝材、制造方法及应用

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 19945357

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 19945357

Country of ref document: EP

Kind code of ref document: A1