WO2021023284A1 - 高钪含量铝钪合金靶材及其制备方法 - Google Patents

高钪含量铝钪合金靶材及其制备方法 Download PDF

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WO2021023284A1
WO2021023284A1 PCT/CN2020/107596 CN2020107596W WO2021023284A1 WO 2021023284 A1 WO2021023284 A1 WO 2021023284A1 CN 2020107596 W CN2020107596 W CN 2020107596W WO 2021023284 A1 WO2021023284 A1 WO 2021023284A1
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scandium
aluminum
alloy target
scandium alloy
content according
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PCT/CN2020/107596
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English (en)
French (fr)
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刘华
黄美松
樊玉川
王志坚
贾帅广
傅臻
姚茂海
杨露辉
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湖南稀土金属材料研究院
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Priority to US17/633,837 priority Critical patent/US20220228240A1/en
Publication of WO2021023284A1 publication Critical patent/WO2021023284A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/02—Compacting only
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/1003—Use of special medium during sintering, e.g. sintering aid
    • B22F3/1007—Atmosphere
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/17—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by forging
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/18—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by using pressure rollers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • 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
    • C22C1/026—Alloys based on aluminium
    • 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
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • 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
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/24—After-treatment of workpieces or articles
    • B22F2003/248—Thermal after-treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps

Definitions

  • the application relates to the technical field of aluminum alloy target material processing and preparation, in particular to an aluminum-scandium alloy target material with high scandium content and a preparation method thereof.
  • Thin film materials are the key support for the manufacture of electronic devices.
  • aluminum thin films have become key materials in the fields of integrated circuits, discrete devices, and liquid crystal displays due to their low resistivity, easy deposition, easy etching, and mature technology.
  • electronic information technology in the direction of high-performance, multi-function, large-capacity, and miniaturization, the integration of semiconductor chips has become higher and higher, and the width of integrated circuit metal interconnections has continued to decrease.
  • High-purity aluminum metal interconnections are electrically connected during use. The problem of migration and stress migration is outstanding, and it has been unable to meet the continuous development of the miniaturization of electrode wiring.
  • Chinese Patent CN107841639A discloses a method for preparing aluminum-scandium alloy target blanks, and its preparation method and application, and specifically discloses the use of powder sintering method to prepare aluminum-scandium alloy containing 0.1%-15% scandium Target blank.
  • Chinese Patent CN 108441827A discloses a method for preparing an aluminum-scandium alloy target material, and specifically discloses the use of a powder sintering method to prepare an aluminum-scandium alloy target blank containing 2% to 50% of scandium.
  • Chinese Patent CN106086567 (Publication Date 2016.11.09) discloses an aluminum-scandium alloy with high scandium content and a preparation method thereof, and specifically discloses the use of a powder sintering method to prepare an aluminum-scandium alloy containing 55% to 70% scandium; wherein the method will The aluminum powder and scandium powder above 99.5% are pre-compacted at room temperature and put into a vacuum hot press to be sintered to prepare a target material containing 2%-50% scandium.
  • the above-mentioned preparation methods disclosed in the prior art all require expensive metal powders as raw materials, and the cost is relatively high, and the metal scandium powder and aluminum powder are easily oxidized, and the oxygen content is relatively high, which affects the purity of the product.
  • powder metallurgy can prepare aluminum-scandium alloys with high scandium content, there are many pores in the powder sintered alloy. Although the overall material is very dense, these pores will still cause many disadvantages to the target sputtering process and the quality of the film. Impact.
  • the Chinese patent CN104805406A discloses an aluminum scandium rotating target and a preparation method thereof, and specifically discloses the use of an arc spray method to spray an alloy bottom layer on a stainless steel substrate containing an alloy bottom layer
  • a controlled atmosphere cold spray method is used to spray aluminum scandium powder to prepare a rotating target; the thickness of the aluminum scandium rotating target prepared by the above method is only 3-15mm, and the density is 97%. Its use range is also limited, that is, the application has limitations .
  • this application provides an aluminum-scandium alloy target with high scandium content and a preparation method thereof.
  • the present application provides a method for preparing an aluminum-scandium alloy target with a high scandium content, including:
  • the aluminum-scandium alloy target blank obtained by sintering is subjected to hot deformation processing to obtain an aluminum-scandium alloy target material.
  • the hot deformation processing includes hot forging, hot rolling, and finishing.
  • the aluminum-scandium alloy target blank is sequentially subjected to hot forging, hot rolling, and finishing operations.
  • metal aluminum with a purity of 99.99% or more and metal scandium with a purity of 99.9% or more are selected, and the mass percentage content of the metal scandium is 35%-80%, and the mass percentage content of the metal aluminum is 20%-65%.
  • the smelting process is performed under the protection of vacuum or inert gas. More preferably, each smelting is kept for about 10 minutes, and then cooled, and the next step of doping with aluminum and smelting is performed.
  • the ball milling time of the aluminum-scandium alloy is 0.5-4 h, and the alloy powder with a particle size of less than 300 ⁇ m is obtained by vacuum drying.
  • the alloy powder and lubricant are first stirred in a mixer, and then a hydraulic press is used to maintain the pressure at 35 KN for 5 minutes to obtain an aluminum-scandium alloy green body; in the vacuum sintering step, The aluminum-scandium alloy green billet obtained by pre-compression is sintered at 800-1100° C. in a vacuum or an inert atmosphere for 60-300 minutes, thereby obtaining the aluminum-scandium alloy target billet.
  • the aluminum-scandium alloy target blank obtained by sintering is forged after being kept at 550°C to 800°C for 30 to 45 minutes; wherein the deformation amount does not exceed 30%.
  • the forged target blank is subjected to hot rolling processing at 450°C to 600°C, and annealed after multiple passes of rolling, and then the target is flattened while it is hot, wherein each pass
  • the amount of deformation is 2% to 12%.
  • finishing step finishing the flattened target blank to obtain an aluminum-scandium alloy target material, wherein the thickness of the aluminum-scandium alloy target material is 5-20 mm.
  • the thickness of the aluminum-scandium alloy target material is 10-16 mm.
  • the scandium content in the aluminum-scandium alloy target material is 35% to 80%.
  • the present application provides an aluminum-scandium alloy target with a high scandium content, which is prepared according to the above-mentioned method for preparing an aluminum-scandium alloy target with a high scandium content.
  • the thickness of the aluminum-scandium alloy target material is 10-16 mm.
  • the relative density of the aluminum-scandium alloy target material is greater than 99.0%.
  • the scandium content in the aluminum-scandium alloy target material is 35% to 80%.
  • the present application adopts alloying smelting-powder metallurgy-hot deformation processing technology to prepare aluminum-scandium alloy target material, through alloying smelting, the composition uniformity of the high-scandium content alloy (the scandium content of the aluminum-scandium alloy is 35% to 80%) is ensured.
  • the thermal deformation processing further eliminates the shrinkage cavity, porosity and other defects, so that the obtained aluminum-scandium alloy target has a high relative density, which can reach more than 99.0%; the structure and chemical composition are improved. Uniform, finer grain size and higher ductility.
  • This method can prepare targets with a wide range of ingredients and large sizes, and this method solves the problem that the alloy is brittle and cannot be smelted and casted after the target is processed. It is easy to produce on a large scale and can meet the needs of a new generation of very large scale integrated circuits. Wiring materials require large-size targets, which can save raw material costs and protect the environment.
  • a preferred embodiment of the present application provides a method for preparing an aluminum-scandium alloy target with a high scandium content.
  • the method includes alloying smelting, powder making, pre-pressing, vacuum sintering, hot forging, hot rolling, and machining steps. Specifically, it includes the following steps:
  • Alloying smelting select metal aluminum with a purity of 99.99% or more and metal scandium with a purity of 99.9% or more, and the mass percentage content of metal scandium is 35% to 80%, and the mass percentage content of metal aluminum is 20% to 65%.
  • the metal scandium is first melted, and then the metal aluminum is gradually added to the metal scandium, smelted and cooled for many times, to obtain an aluminum-scandium alloy.
  • the metal aluminum is divided into multiple parts, each time one part of the metal aluminum is added, and the heat is kept for about 10 minutes, and then cooled, and then the next part of the metal aluminum is added for smelting, heat preservation, and cooling operations.
  • the scandium content in the obtained aluminum scandium alloy is 35% to 80%.
  • Pre-pressing first stir the alloy powder and lubricant in a mixer, and use a hydraulic press to maintain the pressure at 35KN for 5 minutes to obtain an aluminum-scandium alloy green body.
  • Vacuum sintering the green body is sintered in a vacuum or an inert atmosphere at 800 to 1100°C for 60 to 300 minutes to obtain an aluminum-scandium alloy target.
  • Hot forging the target blank obtained by sintering is held at 550°C to 800°C for 30 to 45 minutes and then forged, with a deformation not exceeding 30%, and then annealed.
  • Hot rolling Hot rolling the target blank obtained above at 450°C to 600°C, with a deformation of 2% to 12% per pass, annealing after multiple passes, and finally taking advantage of the aluminum scandium target Heat leveling.
  • the target blank obtained above is processed by a lathe and a machining center to obtain an aluminum-scandium alloy target of the required specification.
  • the thickness of the obtained aluminum-scandium alloy target may be 5-20 mm.
  • the required specifications can be for example And other different specifications.
  • metal aluminum is added to the metal scandium for smelting to ensure the uniformity of the composition of the high scandium content alloy; powder preparation, pre-pressing and sintering reduce the shrinkage cavity, porosity and other defects in the alloy, saving The cost of raw materials is reduced; hot forging, hot rolling and hot deformation processing technology of machining further eliminates the shrinkage and looseness of aluminum-scandium alloy target blanks, so that the obtained aluminum-scandium alloy target has a high relative density, which can reach 99.0% the above.
  • the structure and chemical composition of the aluminum-scandium alloy target obtained by the above-mentioned embodiments are more uniform, the grain size is smaller, and the ductility is higher, which is beneficial for subsequent applications.
  • the foregoing embodiments can prepare targets with a wide range of ingredients and large sizes.
  • the green body was vacuum sintered at 850°C for 60 minutes to obtain an aluminum-scandium alloy target blank.
  • the target blank obtained by sintering is subjected to hot deformation processing. First, it is forged after holding at 700°C for 45 minutes, and the deformation does not exceed 30%. After annealing, it is hot rolled at 500°C, and the deformation is 2%-12% per pass. Multi-pass rolling and then annealing treatment, and finally the target blank obtained above is processed by finishing The density of the aluminum-scandium alloy target material measured by the drainage method is 99.28%.
  • the alloy powder and lubricant are stirred in a mixer, put into a mold with a diameter of 250 mm, and kept under pressure at a hydraulic press of 35 KN for 5 minutes to obtain a green aluminum-scandium alloy.
  • the green body was vacuum sintered at 1050°C for 120 minutes to obtain an aluminum-scandium alloy target blank.
  • the target blank obtained by sintering is subjected to hot deformation processing. First, it is forged after holding at 750°C for 30 minutes, and the deformation does not exceed 30%. After annealing, it is hot rolled at 550°C, with a deformation of 2% to 12% per pass. After multi-pass rolling, annealing is performed, and finally the target blank obtained above is processed by finishing
  • the density of the aluminum-scandium alloy target material measured by the drainage method is 99.35%.
  • the green body was vacuum sintered at 800°C for 210min to obtain aluminum-scandium alloy target blank.
  • the target blank obtained by sintering is subjected to hot deformation processing. First, it is forged after holding at 650°C for 30 minutes, and the deformation does not exceed 30%. After annealing, it is hot rolled at 450°C with a deformation of 2% to 12% per pass. After multi-pass rolling, annealing is performed, and finally the target blank obtained above is processed by finishing The density of the aluminum-scandium alloy target material measured by the drainage method is 99.45%.
  • the green body was vacuum sintered at 900°C for 240 minutes to obtain an aluminum-scandium alloy target blank.
  • the target blank obtained by sintering is subjected to hot deformation processing. First, it is forged after holding at 700°C for 30 minutes, and the deformation does not exceed 30%. After annealing, it is hot rolled at 500°C with a deformation of 2% to 12% per pass. After multi-pass rolling, annealing is performed, and finally the target blank obtained above is processed by finishing The density of the aluminum-scandium alloy target material measured by the drainage method is 99.68%.
  • the green body was vacuum sintered at 800°C for 240 minutes to obtain an aluminum-scandium alloy target blank.
  • the target blank obtained by sintering is subjected to hot deformation processing. First, it is forged after holding at 650°C for 30 minutes, and the deformation does not exceed 30%. After annealing, it is hot rolled at 450°C with a deformation of 2% to 12% per pass. After multi-pass rolling, annealing is performed, and finally the target blank obtained above is processed by finishing The density of the aluminum-scandium alloy target material measured by the drainage method is 99.68%.

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Abstract

本申请公开了一种高钪含量铝钪合金靶材及其制备方法。其中方法包括：选取金属铝和金属钪，并配料；将金属钪熔化，然后将金属铝分多次逐步加入到金属钪中熔炼，多次熔炼后冷却得到铝钪合金；将所述铝钪合金进行球磨，真空干燥得到合金粉，然后经预压制和真空烧结得到铝钪合金靶坯；将得到的铝钪合金靶坯进行热变形加工，得到铝钪合金靶材，所述热变形加工包括热锻、热轧、以及精加工。采用本申请使得铝钪合金靶材组织和化学成分更均匀，相对密度更高，达到99.0％以上，晶粒尺寸更细小，延展性更高；采用本申请还减少了缩孔、疏松缺陷；节省了原料成本；解决了合金脆性大，不能加工靶材的难题；可满足大规模集成电路用配线材料的需求。

Description

高钪含量铝钪合金靶材及其制备方法
本申请要求于2019年08月08日提交的中国专利申请No.201910728801.2的优先权和权益，其全部内容通过引用结合在本申请中。
技术领域
本申请涉及铝合金靶材加工制备技术领域，特别是涉及一种高钪含量铝钪合金靶材及其制备方法。
背景技术
薄膜材料是电子器件制造的关键支撑，其中铝薄膜由于具有电阻率较低、易沉积、易刻蚀、工艺成熟等优点，成为集成电路、分立器件、液晶显示等领域的关键材料。随着电子信息技术向高性能、多功能、大容量、微型化方向发展，半导体芯片集成度越来越高，集成电路金属互联线宽度不断减小，高纯铝金属互联线在使用过程中电迁移和应力迁移问题突出，已无法满足电极布线微细化的不断发展。为了解决纯铝互联线在使用过程中出现的电迁移和应力迁移问题，高技术用铝靶材逐渐向合金化、多元化发展。金属钪在铝合金中具有细化晶粒、抑制合金再结晶、改善抗蚀性等作用，可显著提高合金的强度、塑性、高温性能、抗蚀性能及焊接性能等，有研究发现铝钪合金靶材沉积而成的铝钪薄膜不仅能保持与高纯铝相当的电导率，而且能提高耐腐蚀性，特别是可以显著抑制电迁移和应力迁移。因此，铝钪合金靶材被认为是新一代极大规模集成电路用配线材料。
现有技术中公开的采用铝热还原法或电解法制备铝钪合金的方法，都仅限于低钪含量的铝钪中间合金的制备，且制备过程中存在杂质引入，局限性大的问题。
现有技术中公开了采用粉末烧结法制备铝钪合金的方法。例如：中国专利CN107841639A(公开日2018.03.27)公开了一种铝钪合金靶坯制备方法及 其制备方法及应用，并具体公开了采用粉末烧结法制得含钪0.1％～15％的铝钪合金靶坯。中国专利CN 108441827A(公开日2018.08.24)公开了一种铝钪合金靶材制备方法，并具体公开了采用粉末烧结法制得含钪2％～50％的铝钪合金靶坯。中国专利CN106086567(公开日2016.11.09)公开了一种高钪含量铝钪合金及其制备方法，并具体公开了采用粉末烧结法制得含钪55％～70％的铝钪合金；其中该方法将99.5％以上铝粉和钪粉在室温下进行预压紧，放入真空热压机中烧结制备成含钪2％～50％的靶材。然而，上述现有技术公开的制备方法均需以价格昂贵的金属粉末为原料，成本较高，且金属钪粉和铝粉易氧化，含氧量较高，影响制品的纯度。而且粉末冶金法虽然可以制备高钪含量的铝钪合金，但粉末烧结的合金中有许多的孔隙，尽管材料整体十分致密，但这些孔隙仍会对靶材溅射过程及成膜质量产生许多不利的影响。
现有技术中的中国专利CN104805406A(公开日2015.07.29)公开了一种铝钪旋转靶材及其制备方法，并具体公开了采用电弧喷涂方法喷涂合金底层，在含有合金打底层的不锈钢基体上使用可控气氛冷喷涂方法喷涂铝钪粉末制备旋转靶材；通过以上方法制备的铝钪旋转靶材厚度只有3～15mm，致密度97％，其使用范围也受到了限制，即应用具有局限性。
因此，寻找一种高纯度、低偏析、高性能、低成本且环保的铝钪合金靶材的制备方法显得尤为重要，特别是钪含量越高的铝钪靶材的加工性能越差，所以高钪含量的铝钪合金靶材的制备方法成为人们研究的重点。
发明内容
针对上述问题，本申请提供一种高钪含量铝钪合金靶材及其制备方法。
本申请采用的技术方案如下：
根据本申请一个方面，本申请提供一种高钪含量铝钪合金靶材的制备方法，包括：
选取金属铝和金属钪，并进行配料；将金属钪熔化，然后将金属铝分多次逐步加入到金属钪中进行熔炼，多次熔炼并冷却，得到铝钪合金；
将所述铝钪合金进行球磨，真空干燥得到合金粉，然后经预压制，以及真空烧结，得到铝钪合金靶坯；
将烧结得到的铝钪合金靶坯进行热变形加工，得到铝钪合金靶材，所述热变形加工包括热锻、热轧、以及精加工。
优选地，将铝钪合金靶坯依次进行热锻、热轧、以及精加工操作。
优选地，选取纯度99.99％以上的金属铝和纯度99.9％以上的金属钪，按金属钪的质量百分比含量为35％～80％，金属铝的质量百分比含量为20％～65％配料。
优选地，所述熔炼过程是在真空或者惰性气体保护下进行。更优选地，每次熔炼保温10min左右，然后冷却，进行下一次掺金属铝及熔炼步骤。
优选地，所述铝钪合金的球磨时间为0.5～4h，真空干燥得到粒径小于300μm的合金粉。
优选地，所述预压制步骤中，先将所述合金粉与润滑剂在混料机中搅拌，再使用液压机在35KN下保压5min，得到铝钪合金生坯；所述真空烧结步骤中，将预压制得到的铝钪合金生坯在800～1100℃下，真空或惰性气氛中在烧结60～300min，从而得到所述铝钪合金靶坯。
优选地，所述热锻步骤中，将烧结得到的铝钪合金靶坯在550℃～800℃下保温30～45min后进行锻造；其中，变形量不超过30％。
优选地，所述热轧步骤中，将锻造后的靶坯在450℃～600℃下进行热轧加工，多道次轧制后退火，接着将靶材趁热整平，其中，每道次变形量2％～12％。
优选地，所述精加工步骤中，对整平后的靶坯精加工，得到铝钪合金靶材，其中，所述铝钪合金靶材的厚度为5～20mm。
进一步地，所述铝钪合金靶材的厚度为10～16mm。
优选地，所述铝钪合金靶材中钪含量为35％～80％。
根据本申请的另一个方面，本申请提供的一种高钪含量铝钪合金靶材， 所述铝钪合金靶材是根据上述的高钪含量铝钪合金靶材的制备方法制备得到。
优选地，所述铝钪合金靶材的厚度为10～16mm。
优选地，所述铝钪合金靶材的相对密度大于99.0％。
优选地，所述铝钪合金靶材中钪含量为35％～80％。
本申请采用合金化熔炼-粉末冶金-热变形加工工艺制备铝钪合金靶材，通过合金化熔炼保证了高钪含量合金(铝钪合金中钪含量为35％～80％)的成分均匀性，通过预压制-烧结减少了缩孔、疏松等缺陷；通过热变形加工进一步消除缩孔、疏松等缺陷，使得得到的铝钪合金靶材相对密度高、可达到99.0％以上；组织和化学成分更均匀，晶粒尺寸更细小，延展性更高。该方法可以制备成分范围广、尺寸大的靶材，而且该方法解决了合金脆性大，不能熔炼铸锭后进行靶材加工的难题，易于规模化生产，可以满足新一代极大规模集成电路用配线材料对大尺寸靶材的需求，且可节省原料成本，保护环境。
具体实施方式
下面将结合本申请实施例对本申请技术方案进行清楚、完整地描述：
本申请一个优选实施例，提供一种高钪含量铝钪合金靶材的制备方法，该方法包括合金化熔炼、制粉、预压制、真空烧结、热锻、热轧以及机加工步骤。具体地，包括如下步骤：
(1)合金化熔炼：选取纯度99.99％以上的金属铝和纯度99.9％以上的金属钪，按金属钪的质量百分比含量为35％～80％、金属铝的质量百分比含量为20％～65％，在真空和/或保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加入到金属钪中，多次熔炼，冷却，得到铝钪合金。其中，将金属铝分为多份，每次加入一份金属铝后熔炼保温10min左右，然后冷却，再加入下一份金属铝进行熔炼、保温、及冷却操作。其中，得到的铝钪合金中钪含量为35％～80％。
(2)制粉：将铝钪合金以酒精为介质，球磨0.5～4h后，真空干燥得到 300μm以下的合金粉。
(3)预压制：先将合金粉与润滑剂在混料机中搅拌，使用液压机在35KN下保压5min，得到铝钪合金生坯。
(4)真空烧结：将生坯在800～1100℃下，真空或惰性气氛中在烧结60～300min，得到铝钪合金靶坯。
(5)热锻：将烧结得到的靶坯在550℃～800℃保温30～45min后进行锻造，变形量不超过30％，然后退火。
(6)热轧：将上述得到的靶坯在450℃～600℃下进行热轧加工，每道次变形量2％～12％，多道次轧制后退火，最后将铝钪靶材趁热整平。
(7)机加工：将上述得到靶坯采用车床以及加工中心精加工，得到所需规格的铝钪合金靶材。其中，得到的铝钪合金靶材的厚度可以为5～20mm。所需规格例如可以为
Figure PCTCN2020107596-appb-000001
Figure PCTCN2020107596-appb-000002
等不同规格。
上述实施例通过将金属铝分多次加入到金属钪中进行熔炼，保证了高钪含量合金的成分均匀性；通过制粉末和预压制以及烧结减少了合金中的缩孔、疏松等缺陷，节省了原料成本；通过热锻和热轧以及机加工的热变形加工工艺进一步消除了铝钪合金靶坯的缩孔、疏松等缺陷，使得得到的铝钪合金靶材相对密度高、可达到99.0％以上。通过上述实施例得到的铝钪合金靶材的组织和化学成分更均匀，晶粒尺寸更细小，延展性更高，有利于后续应用。另外，上述实施例可以制备成分范围广，尺寸大的靶材。
实施例1
选取纯度99.99％的金属铝820g和纯度99.9％的金属钪455.3g，在保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加到金属钪中，多次熔炼冷却后得到钪含量35.7％的铝钪合金；将铝钪合金以酒精为介质，球磨2h后，真空干燥得到300μm以下的合金粉。先将合金粉与润滑剂在混料机中搅拌，装入直径200mm的模具中，在液压机35KN下保压5min，得到铝钪合 金生坯。将生坯在850℃下，真空烧结60min，得到铝钪合金靶坯。将烧结得到的靶坯进行热变形加工，首先700℃保温45min后进行锻造，变形量不超过30％，退火后，在500℃下进行热轧加工，每道次变形量2％～12％，多道次轧制再进行退火处理，最后将上述得到靶坯精车加工得到
Figure PCTCN2020107596-appb-000003
的铝钪合金靶材，采用排水法测量致密度为99.28％。
实施例2
选取纯度99.99％的金属铝800g和纯度99.9％的金属钪665.2g，在保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加到金属钪中，多次熔炼冷却后得到钪含量45.4％的铝钪合金；将铝钪合金以酒精为介质，球磨2h后，真空干燥得到300μm以下的合金粉。先将合金粉与润滑剂在混料机中搅拌，装入直径250mm的模具中，在液压机35KN下保压5min，得到铝钪合金生坯。将生坯在1050℃下，真空烧结120min,得到铝钪合金靶坯。将烧结得到的靶坯进行热变形加工，首先750℃保温30min后进行锻造，变形量不超过30％，退火后，在550℃下进行热轧加工，每道次变形量2％～12％，多道次轧制后再进行退火处理，最后将上述得到靶坯精车加工得到
Figure PCTCN2020107596-appb-000004
的铝钪合金靶材，采用排水法测量致密度为99.35％。
实施例3
选取纯度99.99％的金属铝600g和纯度的99.9％的金属钪733.3g，在保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加到金属钪中，多次熔炼冷却后得到钪含量55％的铝钪合金；将铝钪合金以酒精为介质，球磨3h后，真空干燥得到300μm以下的合金粉。先将合金粉与润滑剂在混料机中搅拌，装入直径200mm的模具中，在液压机35KN下保压5min，得到铝钪合金生坯。将生坯在800℃下，真空烧结210min,得到铝钪合金靶坯。将烧结得到的靶坯进行热变形加工，首先650℃保温30min后进行锻造，变形量不超过30％，退火后，在450℃下进行热轧加工，每道次变形量2％～12％，多道次轧制后再进行退火处理，最后将上述得到靶坯精车加工得到
Figure PCTCN2020107596-appb-000005
的铝 钪合金靶材，采用排水法测量致密度为99.45％。
实施例4
选取纯度99.99％的金属铝600g和纯度99.9％的金属钪1000g，在保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加到金属钪中，多次熔炼冷却后得到钪含量62.5％的铝钪合金；将铝钪合金以酒精为介质，球磨3h后，真空干燥得到300μm以下的合金粉。先将合金粉与润滑剂在混料机中搅拌，装入直径200mm的模具中，在液压机35KN下保压5min，得到铝钪合金生坯。将生坯在900℃下，真空烧结240min,得到铝钪合金靶坯。将烧结得到的靶坯进行热变形加工，首先700℃保温30min后进行锻造，变形量不超过30％，退火后，在500℃下进行热轧加工，每道次变形量2％～12％，多道次轧制后再进行退火处理，最后将上述得到靶坯精车加工得到
Figure PCTCN2020107596-appb-000006
的铝钪合金靶材，采用排水法测量致密度为99.68％。
实施例5
选取纯度99.99％的金属铝300g和纯度99.9％的金属钪998.7g，在保护性气体氛围中，先将金属钪熔化，然后将金属铝分次逐步加到金属钪中，多次熔炼冷却后得到钪含量76.9％铝钪合金；将铝钪合金以酒精为介质，球磨2h后，真空干燥得到300μm以下的合金粉。先将合金粉与润滑剂在混料机中搅拌，装入直径200mm的模具中，在液压机35KN下保压5min，得到铝钪合金生坯。将生坯在800℃下，真空烧结240min,得到铝钪合金靶坯。将烧结得到的靶坯进行热变形加工，首先650℃保温30min后进行锻造，变形量不超过30％，退火后，在450℃下进行热轧加工，每道次变形量2％～12％，多道次轧制后再进行退火处理，最后将上述得到靶坯精车加工得到
Figure PCTCN2020107596-appb-000007
的铝钪合金靶材，采用排水法测量致密度为99.68％。

Claims (14)

  1. 一种高钪含量铝钪合金靶材的制备方法，其中，所述制备方法包括：
    选取金属铝和金属钪，并进行配料；将金属钪熔化，然后将金属铝分多次逐步加入到金属钪中熔炼，多次熔炼并冷却，得到铝钪合金；
    将所述铝钪合金进行球磨，真空干燥得到合金粉，然后经预压制和真空烧结，得到铝钪合金靶坯；
    将烧结得到的铝钪合金靶坯进行热变形加工，得到铝钪合金靶材，所述热变形加工包括热锻、热轧、以及精加工。
  2. 根据权利要求1所述的高钪含量铝钪合金靶材的制备方法，其中，选取纯度99.99％以上的金属铝和纯度99.9％以上的金属钪，按金属钪的质量百分比含量为35％～80％，金属铝的质量百分比含量为20％～65％配料。
  3. 根据权利要求2所述的高钪含量铝钪合金靶材的制备方法，其中，所述熔炼过程是在真空或者惰性气体保护下进行。
  4. 根据权利要求1所述的高钪含量铝钪合金靶材的制备方法，其中，所述球磨时间为0.5～4h，真空干燥得到粒径小于300μm的合金粉。
  5. 根据权利要求4所述的高钪含量铝钪合金靶材的制备方法，其中，所述预压制和真空烧结步骤中，先将所述合金粉与润滑剂在混料机中搅拌，再使用液压机在35KN下保压5min，得到铝钪合金生坯；将预压制得到的铝钪合金生坯在800～1100℃下，真空或惰性气氛中烧结60～300min。
  6. 根据权利要求1所述的高钪含量铝钪合金靶材的制备方法，其中，所述热锻步骤中，将烧结得到的铝钪合金靶坯在550℃～800℃下保温30～45min后进行锻造；其中，变形量不超过30％。
  7. 根据权利要求6所述的高钪含量铝钪合金靶材的制备方法，其中，所述热轧步骤中，将锻造后的靶坯在450℃～600℃下进行热轧加工，多道次轧制后退火，接着将靶材趁热整平，其中，每道次变形量2％～12％。
  8. 根据权利要求1所述的高钪含量铝钪合金靶材的制备方法，其中，所 述精加工步骤中，对整平后的靶坯精加工，得到铝钪合金靶材，其中，所述铝钪合金靶材的厚度为5～20mm。
  9. 根据权利要求8所述的高钪含量铝钪合金靶材的制备方法，其中，所述铝钪合金靶材的厚度为10～16mm。
  10. 根据权利要求1所述的高钪含量铝钪合金靶材的制备方法，其中，所述铝钪合金靶材中钪含量为35％～80％。
  11. 一种高钪含量铝钪合金靶材，其中，所述铝钪合金靶材根据权利要求1所述的高钪含量铝钪合金靶材的制备方法制备得到。
  12. 根据权利要求11所述的高钪含量铝钪合金靶材，其中，所述铝钪合金靶材的厚度为10～16mm。
  13. 根据权利要求11所述的高钪含量铝钪合金靶材，其中，所述铝钪合金靶材的相对密度大于99.0％。
  14. 根据权利要求11所述的高钪含量铝钪合金靶材，其中，所述铝钪合金靶材中钪含量为35％～80％。
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