WO2021046929A1 - Cible rotative de ni-cr de grand diamètre contenant des éléments de trace et son procédé de préparation - Google Patents

Cible rotative de ni-cr de grand diamètre contenant des éléments de trace et son procédé de préparation Download PDF

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Publication number
WO2021046929A1
WO2021046929A1 PCT/CN2019/108215 CN2019108215W WO2021046929A1 WO 2021046929 A1 WO2021046929 A1 WO 2021046929A1 CN 2019108215 W CN2019108215 W CN 2019108215W WO 2021046929 A1 WO2021046929 A1 WO 2021046929A1
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WO
WIPO (PCT)
Prior art keywords
diameter
rotating target
trace elements
containing trace
target containing
Prior art date
Application number
PCT/CN2019/108215
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English (en)
Chinese (zh)
Inventor
吴宇宁
卿海标
周其刚
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南京达迈科技实业有限公司
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Publication of WO2021046929A1 publication Critical patent/WO2021046929A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C37/00—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape
    • B21C37/06—Manufacture of metal sheets, bars, wire, tubes or like semi-manufactured products, not otherwise provided for; Manufacture of tubes of special shape of tubes or metal hoses; Combined procedures for making tubes, e.g. for making multi-wall tubes
    • 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
    • C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
    • C22C19/058—Alloys based on nickel or cobalt based on nickel with chromium without Mo and W
    • 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
    • C22F1/002—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working by rapid cooling or quenching; cooling agents used therefor
    • 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-Cr rotating target material containing trace elements and a preparation method thereof.
  • One of the objectives of the present invention is to provide a large-diameter Ni-Cr rotating target material containing trace elements.
  • the addition of trace elements enables the alloy to be effectively fed during the later stage of solidification, reducing the area of defect formation, and It can inhibit the initiation of cracks, improve the bonding force of the grain boundary, and refine the grains, thereby increasing the yield;
  • the second purpose of the present invention is to improve the preparation method of a large-diameter Ni-Cr rotating target containing trace elements.
  • the obtained rotating target material has high utilization rate, can be applied to special coating industry, and can overcome the problems of nickel-chromium tube cracking, inclusions, defects, eccentricity and processing difficulties during the preparation process.
  • the content of Fe as an impurity in the rotating target is less than 0.01%.
  • Impurity iron has the greatest impact on the target magnetron sputtering, so the appropriate raw material composition ratio and preparation process are adopted to reduce the impurity iron content in the rotating target.
  • the present invention also provides a method for preparing the large-diameter Ni-Cr 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, including photoelectric carbon with purity ⁇ 99.9%, boron particles with purity ⁇ 99.5%, metallic zirconium with purity ⁇ 99.5%, metallic magnesium or nickel-magnesium intermediate alloy with purity ⁇ 99.9%, purity ⁇ 99.43% metallic chromium, 99.96% electrolytic nickel; then the raw materials are mixed with electrolytic nickel, metallic chromium, and photoelectric carbon according to the content of the above components, and then vacuum smelted at 1400 ⁇ 1550°C for 70 ⁇ 90min, and then zirconium is added , Magnesium or nickel-magnesium master alloy and boron are refined for 10-20 minutes, and then cast in a protective atmosphere to obtain an ingot; wherein the vacuum degree is maintained at less than 4Pa during the entire 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 1100 ⁇ 1300°C, and after holding for 20 ⁇ 50min, forging is carried out, the forging temperature is 1100 ⁇ 1300°C, and the final forging temperature is 950 ⁇ 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 1100-1200°C; then the hole is expanded at a speed of 150-220mm/s; then a secondary induction is used Heat treatment, the heating temperature is 1110-1220 DEG C, and the hot extruder is used for extrusion, and the extrusion speed is 120-150mm/s, to obtain the waste tube of the rotating target.
  • the waste tube can be processed to an outer diameter of 170-200mm, an inner diameter of 130-160mm, and a length of 2500-4500mm; it can also be adjusted according to the actual needs of the final target processed.
  • the pickling treatment pickling the waste pipe 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 550-650°C for 5-8 hours. Long-term baking can effectively remove most of the hydrogen contained in electrolytic nickel.
  • zirconium, magnesium, and boron are added in the vacuum melting process by enclosing the zirconium, magnesium, and boron by nickel foil; and the trace alloy elements metal zirconium and metal magnesium are added in the vacuum melting process in the above manner.
  • Boron particles can avoid boiling and sputtering of molten steel caused by direct addition.
  • the waste pipe is heated to 1000-1100° 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.
  • Electrolytic nickel can effectively remove the hydrogen contained in electrolytic nickel through long-term high-temperature baking; through repeated thickening and elongation forging process, reaming after induction heating and extrusion, finishing rolling or finishing after secondary induction heating Processes such as boring can improve the concentricity and yield rate of the rotating target;
  • Ni-Cr rotating target containing trace elements of the present invention has simple production process, high yield, high precision, low cost, large pipe diameter, and broad application prospects.
  • composition and content of the large-diameter Ni-Cr rotating target in this embodiment are as follows in terms of mass percentage: C 0.04%, B 0.06%, Zr 0.03%, Mg 0.09%, Cr 44% and the balance Ni and Inevitable impurities.
  • Vacuum melting prepare raw materials of photoelectric carbon, boron particles, metal zirconium, metal magnesium, metal chromium, and electrolytic nickel.
  • the raw materials are: photoelectric carbon with a purity of 99.9%, 99.83% boron particles, and 99.9% metal zirconium. 99.9% metallic magnesium, 99.95% metallic chromium, 99.96% electrolytic nickel;
  • the surface oil stains and oxides of electrolytic nickel and metallic chromium are cleaned and dried and weighed. Then, the electrolytic nickel is kept at 600°C for 6 hours and bake; then the raw materials are prepared according to the content of the above components.
  • the electrolytic nickel, metallic chromium Put the photoelectric carbon into a vacuum melting crucible and smelt with electricity. The melting temperature is 1500°C, and the melting time is 80min. Then add the metal zirconium, metal magnesium and boron particles wrapped in nickel foil successively, and then refining for 15min. The whole melting process is vacuum The degree is less than 4Pa; after smelting, the casting is carried out. Before casting, argon gas 4Mpa is passed in a vacuum state, and the casting is carried out under the condition of protective atmosphere. After 40 minutes of casting, the mold is demolded to obtain the ingot.
  • the second machining remove the surface oxide scale of the cylindrical forging rod, and process both ends of the forging rod to be flat to ensure that the end surface is perpendicular to the cylindrical surface. After processing, it will be a cylinder with a diameter of 299 ⁇ 1mm and a length greater than 500mm. 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;
  • Annealing treatment under the annealing temperature condition of 850°C, heat preservation for 85min for annealing treatment;
  • the preparation method of the large-diameter Ni-Cr rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • 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 (9) the annealing temperature is 870°C and the temperature is kept for 90 minutes.
  • the preparation method of the large-diameter Ni-Cr rotating target of this embodiment is basically the same as that of embodiment 1, except that:
  • step (5) the induction heating temperature is 1200°C, and the second induction heating temperature is 1220°C;
  • step (7) the solution treatment is heated to 1100°C;
  • the Ni-Cr rotating targets containing trace elements prepared in Examples 1 to 5 were subjected to ICP chemical composition detection and purity testing, and the results are shown in Table 1 and Table 2 respectively. It can be seen from Table 1 that the actual detection content of chromium is slightly higher than the theoretical content (combined purity and input ratio). Trace elements such as zirconium, boron, magnesium, and carbon are all burnt, especially the content of magnesium is very small, so it is not Influencing the purity of the target material, on the contrary, it purifies some impurities and improves the purity; among them, impurity iron has the greatest influence on the magnetron sputtering of the target material, and the iron content of the rotating target material of the present invention is less than 0.01%.
  • the rotating target of the present invention can maintain the purity above 99.9% through the addition of trace elements and vacuum smelting, and can also prepare a high-purity nickel-chromium rotating target of greater than 99.95%, which satisfies most of the rotating sputtering materials. The purity requirements of the shooting target.

Abstract

UL'invention concerne une cible rotative de Ni-Cr de grand diamètre contenant des éléments de trace, comprenant les composants de matière première suivants en pourcentage en masse : 0,01 à 0,05 % de C, 0,02 à 0,08 % de B, 0,01 à 0,06 % de Zr, 0,05 à 0,1 % de Mg, 7 à 44 % de Cr, et le reste étant du Ni et des impuretés inévitables. L'invention concerne également un procédé de préparation d'une cible rotative de Ni-Cr de grand diamètre contenant des éléments de trace.
PCT/CN2019/108215 2019-09-12 2019-09-26 Cible rotative de ni-cr de grand diamètre contenant des éléments de trace et son procédé de préparation WO2021046929A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN201910869342.X 2019-09-12
CN201910869342.XA CN110484885A (zh) 2019-09-12 2019-09-12 一种含微量元素的大管径Ni-Cr旋转靶材及其制备方法

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WO2021046929A1 true WO2021046929A1 (fr) 2021-03-18

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Publication number Priority date Publication date Assignee Title
CN110484885A (zh) * 2019-09-12 2019-11-22 南京达迈科技实业有限公司 一种含微量元素的大管径Ni-Cr旋转靶材及其制备方法
CN111604651B (zh) * 2020-06-28 2021-10-22 沈阳有色金属加工有限公司 大尺寸高纯铜旋转靶材的制备方法

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EP2662461A1 (fr) * 2012-05-07 2013-11-13 Schmidt + Clemens GmbH & Co. KG Alliage fer-chrome-manganèse-nickel
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
CN105734507A (zh) * 2016-04-05 2016-07-06 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
CN105838925A (zh) * 2015-01-12 2016-08-10 宝钢特钢有限公司 耐高温氧化镍基合金
CN110484885A (zh) * 2019-09-12 2019-11-22 南京达迈科技实业有限公司 一种含微量元素的大管径Ni-Cr旋转靶材及其制备方法

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JP5232492B2 (ja) * 2008-02-13 2013-07-10 株式会社日本製鋼所 偏析性に優れたＮｉ基超合金
CN102352482B (zh) * 2011-09-28 2013-08-28 江苏美特林科特殊合金有限公司 一种金属电阻膜用Ni-Cr-Si溅射靶材的制造方法
CN102922233B (zh) * 2012-10-31 2014-10-15 南京达迈科技实业有限公司 一种Ni-Cr磁控溅射靶材的制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2662461A1 (fr) * 2012-05-07 2013-11-13 Schmidt + Clemens GmbH & Co. KG Alliage fer-chrome-manganèse-nickel
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
CN105838925A (zh) * 2015-01-12 2016-08-10 宝钢特钢有限公司 耐高温氧化镍基合金
CN105734507A (zh) * 2016-04-05 2016-07-06 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
CN110484885A (zh) * 2019-09-12 2019-11-22 南京达迈科技实业有限公司 一种含微量元素的大管径Ni-Cr旋转靶材及其制备方法

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