CN111194359B - 超级合金溅射靶 - Google Patents

超级合金溅射靶 Download PDF

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Publication number
CN111194359B
CN111194359B CN201880042156.2A CN201880042156A CN111194359B CN 111194359 B CN111194359 B CN 111194359B CN 201880042156 A CN201880042156 A CN 201880042156A CN 111194359 B CN111194359 B CN 111194359B
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superalloy
target
powder
composition
layer
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CN201880042156.2A
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CN111194359A (zh
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P·波尔西克
J·拉姆
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Plansee Composite Materials GmbH
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Plansee Composite Materials GmbH
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    • 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
    • C23C14/24—Vacuum evaporation
    • C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
    • C23C14/325—Electric arc evaporation
    • 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
    • C22C1/0433—Nickel- or cobalt-based alloys
    • 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
    • B22F3/02—Compacting only
    • B22F3/087—Compacting only using high energy impulses, e.g. magnetic field impulses
    • 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
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • 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
    • C22C1/047—Making non-ferrous alloys by powder metallurgy comprising intermetallic compounds
    • 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
    • C22C—ALLOYS
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    • C22C19/07—Alloys based on nickel or cobalt based on cobalt
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • C23C14/0036—Reactive sputtering
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    • 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
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    • C23C14/024—Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025—Metallic sublayers
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    • 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
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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    • 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
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Abstract

本发明包括超级合金靶，其中该超级合金靶具有随机晶粒取向的多晶结构，该结构中的平均晶粒尺寸小于20μm，并且该结构中的孔隙率小于10％。此外，本发明包括通过粉末冶金生产制造超级合金靶的方法，其中所述粉末冶金生产从超级合金的合金粉末开始并且包括合金粉末的放电等离子体烧结(SPS)步骤。

Description

超级合金溅射靶
技术领域
本发明涉及超级合金(SA)材料领域，尤其涉及根据权利要求1所述的超级合金溅射靶和根据权利要求11所述的通过粉末冶金生产制造超级合金靶的方法.
技术背景
超级合金展现出若干关键特性：优异的机械强度、抗热蠕变变形、良好的表面稳定性和抗腐蚀性或抗氧化性.晶体结构通常是面心立方奥氏体.此类合金的实例是哈斯特洛伊合金(Hastelloy)、因科内尔合金(Inconel)、瓦斯帕洛伊合金(Waspaloy)、Rene合金、海恩斯(Haynes)合金、因科洛伊合金(Incoloy)、MP98T、TMS合金和CMSX单晶合金。超级合金通过固溶强化而发展高温强度.重要的强化机制是弥散强化，其形成第二相沉淀物，例如γ′和碳化物。由诸如铝和铬之类的元素提供抗氧化性或抗腐蚀性。基本上存在两种类型的超级合金，一种是钴基超级合金，其以钴作为主要金属组分，并以例如C、Cr、W、Ni、Ti、Al、Ir和Ta作为合金元素，另一种且直到今天最重要的类别是镍基超级合金，其以镍作为主要金属组分，并以例如Cr、Fe、Co、Mo、W、Ta、Al、Ti、Zr、Nb、Re、Y、V、C、B或Hf仅作为与该超级合金组一起使用的合金添加剂的一些实例.本发明的一个焦点是在总体上，且尤其针对诸如用于航空和工业燃气轮机(IGT)应用的高压和低压涡轮组件之类的应用来改进超级合金的热性能和磨损性能，由此已经用诸如PWA1483和CM247-DS之类的镍基超级合金进行了若干成功的实验。进一步地，基于铝化物的合金例如钛铝基超级合金(比如γ-TiAl)或形成高温和高耐磨合金的另外铝化物在此理解为超级合金组合物，所述另外铝化物包括Ni-铝化物，例如NiAl(也称为雷尼镍)或NiAl3；Fe-铝化物；Hf-铝化物；Cr-铝化物；Nb-铝化物，例如Nb3Al或NbAl3；Ta-铝化物，例如Ta3Al或TaAl3；Pt-铝化物；Zr-铝化物等。
放电等离子体烧结(SPS)是粉末冶金制造方法，由此优选在真空下在例如两个石墨冲头之间的石墨模具中对粉末组合物加压，并且同时在两个冲头之间施加DC电流或任选的脉冲DC电流以辅助待制造的工件(在本案中为靶)的成形过程。从而，在导电样品(比如超级合金)的情况下，DC电流或脉冲DC电流直接通过石墨模具以及粉末压块。因此，与常规的热压相反，热量的产生是内部的，在常规的热压中，由外部加热元件提供热量.这导致在与常规烧结技术相比更低的烧结温度下实现接近理论密度，并且促进非常高的加热或冷却速率(高达1000K/min)，因此烧结过程通常非常快(在几分钟内)。该过程的一般速度确保其具有使具有纳米尺寸或纳米结构的粉末致密化的潜力，同时避免伴随标准致密化途径的粗化。作为实例，对于此类程序，强度高达1500A且低电压为25V的一系列3ms直流电流脉冲可以直接通过粉末样品和压制工具。
对于在高温下以及在氧化和腐蚀环境中使用的材料的研究是正在进行的针对飞行器、燃气轮机和内燃机应用的努力.尽管最终的利用不同并且在设计和尺寸方面存在不同，但这些工业的趋势正朝向相同的目标，该目标是发动机效率的持续改进，以降低燃料消耗而且符合关于CO2排放的更严格规定。这意味着在较高温度下运行发动机，因此随之而来增加了对在涡轮发动机的不同部分处，在恶劣环境中操作的更坚固、稳定和耐久的基础材料的需求.即使使用最先进的材料(例如超级合金或复合材料)，在通过提高在高操作温度下的抗氧化性、耐磨性、耐侵蚀性和耐腐蚀性来改进组件的寿命的情况下，也不能绕过涂覆技术。尽管事实上好几十年前引入的涂覆技术已经得到充分确立，并且通过使用新的方法和新的涂覆材料而被不断改进，但是在发动机组件上产生的涂层系统要求增加的复杂性。因此，例如层之间的相互作用、表面制备方法、热处理和扩散问题变得越来越重要。此外，由于这些现有技术的限制和不能提供所需的特性，下一代发动机的要求对于这些现有技术来说是相当有挑战性的。燃气轮机中的典型涂层系统由若干层制成，通常由粘合涂层、热生长氧化物(层)和顶部陶瓷层组成.通常通过针对PtAl的扩散工艺、电子束物理气相沉积(EB-PVD)或针对MCrAlY的低压等离子体喷涂(LPPS)来产生用于保护涡轮不被氧化的粘合涂层。粘合涂层和顶部陶瓷层形成所谓的热障涂层(TBC)。顶部陶瓷涂层通过大气等离子体喷涂(APS)作为多孔涂层而产生或通过EB-PVD作为柱状结构涂层而产生.粘合涂层的设计是有挑战性的，因为它必须实现两种复杂的界面：一种针对超级合金基底，以保证宽温度范围的机械稳定性，另一种针对多孔氧化物，以提供优异的氧气屏障。这不仅意味着粘合涂层的智能设计，而且在涂层系统(叠层(layer stack))的制造中还要求高再现性。
公开内容和实施例
因此，目的在于通过避免现有技术方法的缺点来改进并简化超级合金的已知涂覆工艺，所述缺点是例如使用昂贵的涂覆材料(比如PtAl)、以及如果必须施加由具有不同蒸气压的元素组成的涂层，则复杂且难以操作的工艺，例如EB-PVD。另一个目的在于在总体性能方面改进现有涂层，例如克服现有技术涂层系统的局限性和无能.
因此，一个目的在于公开涂覆方法，其包括以下步骤：
-在PVD涂覆单元中提供超级合金(SA)基底；
-提供超级合金(SA)靶作为涂覆单元的电弧蒸发源的阴极；
-向基底提供基底偏压；
-从超级合金靶通过真空电弧沉积在基底的表面上沉积超级合金的界面层(IF-1)；
-向所述涂覆单元供应(provide a supply of)含氧反应性气体；
-通过真空电弧沉积来沉积相同超级合金或不同金属组成的过渡层(TL)，由此通过改变工艺气氛中的反应性气体的分压使该层的氧含量从(IF-1)朝向表面变化，例如通过提高和/或改变反应性气体的分压从(IF-1)朝向表面增加该层的氧含量；
-如同沉积过渡层(TL)的情况，在含有更高浓度的反应性气体的工艺气氛中，通过真空电弧沉积，在过渡层之后沉积屏障层(IF-2)，该屏障层包含比过渡层内更高量的超级合金氧化物或与过渡层内不同的金属氧化物组成.
过渡层内的氧含量的任何变化可通过逐步或渐进(ramp-wise)增加/改变含氧反应性气体的流量和/或通过改变电弧源的功率来执行。通常氧气(O2)气体将用作反应性气体，然而，可以使用任何其它挥发性含氧化合物，如臭氧(O3)或其它.
此类涂覆工艺可通过使用具有与超级合金基本相同组成的超级合金靶来执行。从而，根据待涂覆的超级合金的组成选择用于靶生产的粉末组成，以生产具有与超级合金本身基本相同的组成的靶。在本案中，对于靶(如通过SPS或任何其它粉末冶金方法生产的)，“基本相同的组成”表示由于制造和/或例如EDX测量效应，构成粉末混合物的大约9％或更多的重量百分比的主要元素(以PWA1483作为实例，比如Ni、Co和Cr)相对于原始粉末组成的差异不大于±20％，优选不大于±10％。类似地适用于与反应性或非反应性工艺一起使用的靶，其中对于单一主要组分，与原始粉末组成的差异可稍高.这同样适用于术语“与界面层(IF-1)的组成基本相同的组成”的含义.尤其，Ni粉末、Al粉末、C粉末、Co粉末、Cr粉末、Mo粉末、Ta粉末、Ti粉末和W粉末用于生产阴极真空电弧涂敷用的靶，如下所描述。
或者，也可通过粉碎超级合金固体来生产合适的粉末，并且然后通过SPS或另一种粉末冶金方法形成靶。
在最基本的方法中，相同的超级合金靶用于沉积粘合涂层的所有层，并且氧气用作唯一的工艺气体。
已经进一步证明，例如由于形成较少的液滴和建立完全匹配的IF-1层(例如关于晶体学一致性和对基底的外延生长)，提供主要具有相同晶体结构的靶(这意味着对于镍基超级合金或钴基超级合金而言，fcc晶体靶结构为约80-99％)在工艺稳定性方面是有益的.
在另外实施方案中，提供至少一个具有另外金属组成的另外靶，以沉积具有不同金属组成的过渡层和/或具有不同金属氧化物组成的屏障层(IF-2).这可以通过向涂覆单元提供额外的元素或复合靶来完成。这可以通过与超级合金靶的共起弧和/或通过至少一个具有另外金属组成的靶的独立起弧来完成，由此优选其中两种类型的靶用于沉积各自的涂层的过渡相。因此，选择了具有另外金属组成的靶的组成，以致具有不同金属组成和/或不同金属氧化物组成的层可以从具有另外金属组成的靶单独沉积，或者通过与超级合金靶的共起弧沉积。
另选地，或者甚至与如所提及的具有另外金属组成的靶的使用相结合，可将包含待沉积的另外金属的气态前体引入PVD涂敷单元，与超级合金靶的真空电弧沉积并行，以沉积具有不同金属组成的过渡层和/或具有不同金属氧化物组成的屏障层(IF-2)。可通过使用惰性气体或反应性气体的供应管线或通过单独的管线将此类前体引入到涂覆单元中。
尽管事实上通常过渡层内的至少主要金属组分和IF-2内的主要金属组分的比率将大致相同，但应提及的是，通过例如使具有不同金属组成的两个或更多个靶的共起弧并改变一个或两个靶的各自功率输入，或通过改变一种或多种气态前体的流量或通过分别应用上述方法的混合，使任何金属的比率可在各层之间或甚至在各层内逐步或渐进变化。当形成具有氧化屏障性能的氧化物时，尤其可以应用金属含量的此类变化，在标准TBC设计中，在多孔氧化物沉积之前通过高铝含量表面的高温氧化形成所述氧化物。在此描述的新的PVD粘合涂层设计的目标之一是通过在PVD原位工艺中形成氧化物来代替高温氧化。
在另外实施方案中，界面层(IF-1)沉积有与超级合金基底的晶体结构一致的晶体结构.由此甚至可以沉积与超级合金SA的相应表面位置的晶体结构成镜像的外延生长结构。已经证明，应用于多晶、定向凝固(DS)或单晶(SX)SA表面的此类一致的且尤其是外延生长的晶体结构在抗氧化性和粘附性方面给予整个涂层优异性能。
优选地，在反应性气体气氛中用过剩的氧沉积超级屏障层(IF-2)的合金氧化物和/或不同金属组成的氧化物。氧原子与金属原子的比例(＝过剩)可以是至少1.5或甚至至少5，以从在沉积屏障层(IF-2)时蒸发的超级合金金属和/或不同金属组合物(composition)形成热力学稳定的氧化物，尤其最稳定的氧化物.由此，可以形成包含基本上化学计算量的氧化物的屏障层，尤其是对于超级合金或不同金属组合物的大多数或甚至所有的金属元素和/或合金而言，处于热力学上最稳定的相.此类屏障层(IF-2)显示出致密的柱状结构，与例如沉积在多晶SA表面上的界面层(IF-1)的几乎随机的晶粒取向的多晶结构非常不同。
与屏障层相反，可以在没有任何工艺气体的纯金属蒸气中沉积界面层。
或者，可以向涂覆单元供应惰性气体，以在含有惰性气体的工艺气氛中沉积界面层(IF-1)、过渡层和屏障层(IF-2)中的至少一个。
关于必需的涂覆参数，例如工艺压力、电弧电流和基底偏压，应提及以下内容.
如果不使用惰性气体，则用于沉积界面(IF-1)的工艺压力范围为0.1mPa-100mPa.加入惰性气体的情况下，压力增大到(augmented for)约0.1Pa至5Pa。界面层的另外工艺参数，其中：
超级合金靶的电弧电流：80A至250A；
基底偏压：从-20V到-800V的直流电压和双极脉冲偏压。
在添加和不添加惰性气体的情况下，用于在氧反应性气体中沉积过渡层(TL)的工艺压力范围为0.1Pa到5Pa.通常，在沉积过渡层期间的工艺压力已经从没有任何反应性气体用于沉积界面(IF-1，见上面)的非常低的工艺压力增加到用大量反应性气体沉积屏障层(IF-2)的工艺压力(见下面).用于过渡层的另外工艺参数，其中：
超级合金靶的电弧电流：从80A至200A；
具有另外金属组成的靶的电弧电流：60A至200A；
基底偏压：从-20V到-800DC，以及单极和双极脉冲。
如果不使用惰性气体，则用于沉积屏障层(IF-2)的工艺压力范围在0.1Pa和8Pa之间。在加入惰性气体的情况下，压力增大到约0.2Pa至10Pa。界面层的另外工艺参数，其中：
超级合金靶的电弧电流：60A至200A；
具有另外金属组成的靶的电弧电流：60A至220A；
基底偏压：从-20V到-600V的DC，优选单极或双极脉冲
已经选择具有另外金属组成的靶的组成，以致具有不同金属组成和/或不同金属氧化物成分的层可以从至少一个具有另外金属组成的靶单独沉积，或者通过与至少一个超级合金靶共起弧来沉积。或者或另外地，可以使用含有待沉积于过渡层和/或屏障层中的另外金属中的至少一种的前体。
已经证明，使用已通过粉末冶金工艺生产的超级合金靶对于本发明的方法是有益的.此类方法的实例是热压、热等静压(HIP)且尤其是放电等离子体烧结(SPS)。
本发明涉及超级合金靶的生产，其中：
-超级合金靶具有随机晶粒取向的多晶结构，
-该结构中的平均晶粒尺寸小于20μm，和
-该结构中的孔隙率小于10％.
在本发明的另外实施方案中，超级合金靶的特征在于所述超级合金是以钴作为主要金属组分的钴基超级合金。
在本发明的另外实施方案中，超级合金靶由钴基超级合金制成，该钴基超级合金包含C、Cr、W、Ni、Ti、Al、Ir和Ta中的至少一种元素作为合金元素.
在本发明的另外实施方案中，超级合金靶的特征在于所述超级合金是以镍作为主要金属组分的镍基超级合金.
在本发明的另外实施方案中，超级合金靶由镍基超级合金制成，该镍基超级合金包含Cr、Fe、Co、Mo、W、Ta、Al、Ti、Zr、Nb、Re、Y、V、C、B和Hf中的至少一种元素作为合金元素.
在本发明的另外实施方案中，超级合金靶的特征在于所述超级合金是基于铝化物的合金.
在本发明的另外实施方案中，超级合金靶由基于铝化物的超级合金、钛铝基超级合金、Ni-铝化物、Fe-铝化物、Hf-铝化物、Cr-铝化物、Nb-铝化物、Ta-铝化物、Pt-铝化物或Zr-铝化物制成。
在本发明的另外实施方案中，超级合金靶在晶体学一致性和外延生长方面主要具有相同晶体结构。
在本发明的另外实施方案中，超级合金靶是镍基超级合金或钴基超级合金，其中fcc晶体结构的比例在80-99％的范围内。
在本发明的另外实施方案中，超级合金靶包含具有相似晶格常数的不同金属间相.
在本发明的另外实施方案中，超级合金靶包含沉淀物。
在本发明的另外实施方案中，超级合金靶的特征在于原始靶的XRD图显示主峰，其可以被标示为fcc立方(相)(fcc cubic)，并且操作靶的XRD图显示与原始靶表面所观察到的fcc立方相类似的fcc立方相。
本发明进一步涉及通过粉末冶金生产制造超级合金靶的方法，其中所述粉末冶金生产从超级合金的合金粉末开始并且包括以下步骤：
-所述合金化粉末的放电等离子体烧结(SPS).
在本发明的另外实施方案中，制造超级合金靶的方法的特征在于，在1000-1350℃的温度范围内进行放电等离子体烧结而不牵涉液相的形成。
在本发明的另外实施方案中，制造超级合金靶的方法的特征在于，在粉末的制造期间发生超级合金靶的各相的合成.
在本发明的另外实施方案中，制造超级合金靶的方法的特征在于，在真空下在两个石墨冲头之间的石墨模具中对粉末组合物加压并且同时施加DC电流或脉冲DC电流。
在本发明的另外实施方案中，制造超级合金靶的方法的特征在于通过粉碎超级合金固体来制造合金粉末。
在另外的变型中，在另外工艺步骤中，向屏障层(IF-2)的表面施加进一步优选的多孔陶瓷顶层.
可通过以下技术来施加此类顶层：热喷涂技术例如爆炸喷涂、金属丝电弧喷涂、火焰喷涂、高速氧燃料涂层喷涂(HVOF)、高速空气燃料(喷涂)(HVAF)、温热喷涂、冷喷涂，以及优选等离子体喷涂或真空等离子体喷涂.
进一步公开了生产经涂覆的超级合金工件的方法，其包括如上所描述的涂覆方法。此类工件可以是例如在工业燃气轮机或飞机发动机的高温区域中使用的任何部件，比如涡轮叶片、轮叶或类似物。
进一步公开了超级合金工件，其包含：
-超级合金基底
-直接在超级合金基底的表面上的具有基本上相同的超级合金组成的界面层(IF-1)，随后
-过渡层(TL)，其具有基本上相同的超级合金和超级合金氧化物或不同的金属组成和不同的金属氧化物，由此过渡层的氧含量从IF-1朝向(IF-2)增加
-具有超级合金氧化物或不同金属氧化物的屏障层(IF-2)。
从而IF-1可以具有与超级合金基底表面的晶体结构一致或甚至向其外延生长的晶体结构。
过渡层中的氧含量可从IF-1到IF-2逐步或逐渐增加.
过渡层中的不同金属组成可与基本上相同的超级合金组成相差至少一种另外元素.屏障层的不同金属氧化物的金属组成也可以由至少一种另外金属来区分，所述另外金属将以氧化物的形式存在。
该至少一种另外元素可具有等于或小于1.4的根据鲍林的电负性.此类低电负性通常针对结合氧的可能性高的金属，例如当此类金属分散在具有较少形成氧化物的趋势的固态金属基体中时。此类另外元素可以是镧系元素，优选为La、Er或Yb中的至少一种。
或者，不同的金属组成可以通过至少一种元素的浓度或通过至少一种下列另外元素的浓度和/或添加而不同于超级合金组成：Mg、Al、Cr、Er、Y、Zr、La、Hf、Si.
至少一部分的另外元素可以被氧化并作为固溶体(SS)在晶粒中沉积和/或沿着过渡层(TL)和/或屏障层(IF-2)的晶界沉积为弥散强化氧化物(ODS)。
已知此类具有低电负性的金属(比如碱金属、碱土金属、镧系元素、锕系元素和元素周期系的第3族和第4族(过渡金属)的一些金属)在此类金属沿着多晶固体的晶界定位并被扩散着的氧原子氧化时，易于在固体主基体的晶粒内形成固溶体(SS)或形成氧化物弥散强化(ODS)的固体。从氧化物弥散硬化工艺中已知使用此类热力学稳定的材料(SS和/或ODS)，以通过仅添加少量此类形成氧化物的元素(约2体积％)来强化此类合金，例如超级合金。然而，在已经沉积根据本发明的涂层的情况下，第一次可以证明涂层具有类似的效果。可以显示在过渡层中用部分氧化的超级合金进行SS和/或ODS强化的效果。
过渡层中至少一种金属元素或硅的浓度可以从IF-1向IF-2逐步或逐渐地调节或增加。不同的金属氧化物可以包含以下氧化物中的至少一种或其混合物：
氧化铝、氧化铝-氧化铬、氧化铒、氧化钇、氧化钇-氧化铝、氧化镁-氧化铝、氧化铝-氧化硅、氧化铪-氧化硅.
因此氧化铝或氧化铝-氧化铬可以是包含刚玉晶体结构的Al2O3或(AlCr)2O3，而氧化铒或氧化钇可以是包含立方晶体结构的Er2O3或Y2O3，并且大于55％，优选大于75％的相应晶体结构可以是相应的刚玉或立方晶体结构.
不同的金属氧化物可以包含含铝氧化物，且TL层和域IF-2层可以包含铝液滴或具有高含量金属铝的液滴.
在包含氧化铝-氧化铬的氧化物的情况下，例如呈刚玉结构和/或作为SS或ODS分散在过渡层和/或屏障层中，所述层也可以包含具有高金属铬含量的液滴。
作为实例，为了用于IGT和航空应用，可以在粘合涂层的顶部之上的屏障层(IF-2)的表面上提供陶瓷顶层作为终端层。此类顶层可以制成具有多孔结构，以更好地适应高温应用中的热膨胀。
关于由连续的
-界面层(IF-1)
-过渡层(TL)和
-屏障层(IF-2)
组成的粘合涂层，可以选择以下总涂层厚度：
1μm≤d粘合≤200μm
其中界面层(IF-1)的层厚：
0.01μm≤dIF-1≤20μm
其中过渡层(TL)的层厚：
0.1μm≤dTL≤100μm
其中屏障层(IF-2)的层厚：
1μm≤dIF-2≤50μm
用于航空或IGT应用的随后的热喷涂陶瓷顶层的厚度选择在10μm和3mm之间，并且显示出优异的粘附力和耐磨性。
在下文，提供实施例和附图.应提及，本发明的任何实施方案、修改或实例的任何组合，如果在本说明书或权利要求书中没有明确提及，也认为是本发明的一部分，只要对于本领域的技术人员而言其不能立即被认为是功能失常的。
附图说明
在下文，借助于实验细节和附图以示例性方式描述本发明。图1至8显示以下内容：
图1粘合涂层的层概念和实例；
图2原始靶和操作靶的XRD图；
图3 SA-T表面的显微照片和EBSD；
图4 SA-T表面的TEM图像；
图5 EDX图(mapping)
图6明场和暗场显微照片，线扫描；
图7蓝宝石上图2的XRD类似物
图8叠层：STEM明场，TKD，质量图；
图9 TEM显微照片界面
通过本公开，引入了图1a中所示意图示的层概念。该方法基于形成与块体超级合金基底(SA-S)相同的″基底-相同″界面层(IF-1)和随后的从IF-1到部分或完全氧化的涂层的过渡层(渐变层)，该过渡层终止于第二界面层，这里也称为屏障层(IF-2)。该IF-2可以是氧扩散屏障层和/或多孔氧化物的成核层，当它被用于TBC的设计中时。它也可以是ODS涂层或在超级合金蒸气的氧化期间中所形成的氧化物混合物。在一个工艺中在通常用于物理气相沉积(PVD)的真空条件下合成整个叠层。利用非反应性和反应性电弧蒸发通过原位处理来产生这种涂层设计.
多晶超级合金上的基础粘合涂层的实例示于图1b中，其包含与超级合金基础非常相似或甚至相同的界面，针对氧浓度渐变的过渡层，这意味着氧含量从界面到屏障层增加，屏障层是根据本实例的经氧化的超级合金.
基底以及靶由具有表1第2列中所列举的化学组成的粉末制备.该组成对应于超级合金PWA1483的规格。然而，在约1200℃和30MPa下，通过放电等离子体烧结来制造基底以及靶(PLANSEE Composite Materials GmbH)。因此，该材料有可能不同于通过熔融和铸造生产的工业上使用的块料。在这方面，重要的是要注意：
-结构中的平均晶粒尺寸小于50μm且优选小于20μm，
-粉末冶金生产优选从合金粉末开始而不是从元素粉末的混合物开始，
-由此在粉末的制造期间而不是在SPS方法期间发生相的合成，
-如此制造的靶没有织构(texture)，即，它们表征为随机晶粒取向(例如通过EBSD测量)，这与通过熔融冶金制造的靶非常不同，
-将通过SPS方法制备的结构中的孔隙率调节至小于10％或优选小于5％，
-在1000-1350℃的温度范围内，优选在1100-1300℃的温度范围内进行SPS方法而不牵涉形成液相。
考虑到这一点，如果将该材料用作基底，则我们将进一步将其命名为超级合金基底(SA-S)，如果将其用作用于蒸发的靶，则将其命名为超级合金靶(SA-T)。由该材料生产小盘 并机械加工成SA-S的尺寸(30mm×10mm×5mm)。在相同的方法中，制造SA-T盘
表2列举了在下面讨论的实施例中使用SA-T作为阴极的阴极电弧蒸发中使用的主要工艺参数.在沉积之前，将处理室抽真空到低于0.02Pa，并且执行标准加热和蚀刻步骤，以确保涂层对基底的充分粘附。针对非反应性工艺(仅金属蒸汽)选择45分钟的净沉积时间并针对在氧气中的反应性工艺增加到240分钟.这是由于在纯氧反应性气体中SA-T的蒸发速率降低，分别导致涂层厚度为1.5μm(反应性)和2.2μm(非反应性).使用OerlikonSurface Solutions AG的INNOVA间歇式生产系统，用140A的DC电弧电流(仅在金属蒸气中)或用800sccm氧气的气流(反应过程)操作阴极。将SA-S与蓝宝石基底一起在约550℃的基底温度下涂覆，仅使用一个电弧源进行沉积。在氧气中处理期间，将频率为25kHz、负脉冲长度为36μs和正脉冲长度为4μs的40V对称双极偏压施加到基底上.
在LEO1530扫描电子显微镜(SEM)中分析靶表面。在SEM中通过能量分散X射线光谱(EDX)测量SA-T和SA-S的化学组成。
在Bruker D8Davici衍射仪上对多晶靶材料的抛光切片执行XRD测量，该衍射仪配备有用于产生平行光束的镜和使用Cu-Kα辐射的LynxEye1D检测器.在5-140°之间以2θ/ω模式进行测量。对于相分析，结合使用来自Bruker的软件Difffrac.Eva V4.1与晶体开放数据库(COD)，该数据库是在Journal of Applied Crystallography(应用晶体学杂志)42(2009)726-729中公开的晶体结构的开放访问集合。
在来自Tescan的双FIB FEG-SEM Lyra3中，使用Digiview IV EDAX照相机，在SA-T表面上执行常规电子背散射衍射(EBSD)分析。使用20kV的加速电压和5nA的发射电流.此外，在厚度为约100nm的举起的(liff-out)样品上进行透射EBSD或透射Kikuchi衍射(TKD)，该样品安装在与极片成20°预倾斜角的支架上，工作距离为3mm。电子束条件为30kV和5nA。通过使用30kV和1.5pA Ga离子进行的离子通道对比成像来分析化学偏析。最后在配备有EDAX EDS系统的JEOL JEM 2200fs中通过透射电子显微镜(TEM)分析举起的薄片。
原始靶(阴极)的分析
通过EDX来调查研究通过放电等离子体烧结制造的SA-T的化学组成.由于待分析的元素的数量大并且它们对于该方法的灵敏度不同，因此定量分析是困难的.然而，材料的相似性允许(除了C之外)定性比较。表1显示了所制造的靶的制造态的(as produced)原始表面的结果，其中关于总元素组成的数值在第3列中，且关于粉末组成的差异(Δ)数值在第4列中。除了碳和钽，在组成上与原始粉末相当一致.将通过XRD分析获得的原始靶表面的晶体结构与在非反应性工艺中电弧操作后的靶表面进行比较.图2中显示了2θ/ω扫描.
原始靶的XRD图(虚线)显示若干主峰，其可被标示为的fcc立方(相)(Fm-3m)。针对由组成超级合金的各种元素(表1)观察到的衍射图与该立方晶格匹配.除了单独的元素之外，许多不同的金属间化合物比如Cr2Ni3、Al2.6Ni10.7Ta0.7、Ni0.9Ta0.1、Ni17W3、Co0.87W0.13、Ni3.28Ti0.72、Ni0.85W0.15或CrNi也可以被标引，并且可以被认为是所观察到的fcc相的潜在候选物。在原始靶表面的XRD图中也可以看到强度低于1％的峰.它们可能属于由于表面氧化而形成的氧化钽相的XRD图。XRD图的峰揭示操作靶(实线)具有与针对原始靶表面观察到的类似的fcc立方(Fm-3m)相。然而，操作靶的峰朝向较高的角度稍微移动，这表明晶胞参数a从原始靶的/>降低到操作靶的/>同时，操作靶的峰比原始靶的那些峰窄，这可能是由于靶表面上的再结晶过程和因此形成较大的微晶.来自X射线衍射分析的存在不同金属间化合物的假设与TEM测量的结果一致。它们证实这些超级合金材料确实由不同的金属间化合物组成(见下文)。
图3a中展示了使用20kV电子束电压，利用背散射电子从SEM获得的SA-T表面的显微照片。背散射图像中的对比主要归因于晶粒取向。这通过所调查研究的表面的相应EBSD晶体取向图证实，其在图3b中以黑白(bw)形式显示.EBSD分析表明88％的高角度晶界和12％的低角度晶界以及7％的∑3孪晶(60°@(111))晶界，平均晶粒尺寸为(5.9±3.1)μm。图3a的观察到的背散射图像中的白点在TEM中被识别为富含钛和钽的沉淀物.分别在图4a和4b中的明场和暗场扫描透射电子显微图像中示出了具有不同晶粒的放大截面.图5中给出了这个细节的EDX图.该图显示，Cr(子图5b)、Co(图5c)和Mo(图5g)也在晶粒内一起偏析(segregate).Ni(图5a)、Al(图5h)、Ti(图5e)和Ta(图5d)也是如此.另外，该图建议沉淀物主要由Ta和Ti组成。
如先前所提及的，从制造态的靶和操作靶的表面获得的XRD图可以用fcc相标记，对于fcc相，不同的金属间化合物可能是潜在的候选物(图2)。STEM调查研究支持了这种假设，其中在晶粒内部和晶粒之间观察到化学偏析。图6显示了跨越两个晶界的过渡的明场(6a)和暗场(6b)显微照片的实例。图6a中的箭头表示执行图6c中所示EDX线扫描的位置.仅绘出了主要元素的定性分布并且它在两个所调查研究的晶粒之间显著变化.可观察到Ni/Al和Co/Cr的偏析(segregation)，这与图5中所显示的图非常一致。这是许多类似的线扫描的情况，其表明存在超过一个具有非常类似的晶格常数的FCC相。
靶的分析表明，放电等离子体烧结工艺产生具有几乎随机的晶粒取向的多晶结构的靶材料。另外，该分析证明了存在具有相似晶格常数的不同金属间相并且在所产生的材料中存在沉淀物。
操作靶的分析
在下一步骤中，将制造态的靶用作阴极并通过电弧进行蒸发.在表2中所提及的条件下执行蒸发。在非反应性工艺中，在蒸发期间不使用额外的气体.这种方法放弃了由于与气体原子的多次散射而可能减少液滴在沉积涂层中的并入，然而，它允许保持金属蒸气的较高电离度和较高动能，支持涂层在较高能量下冷凝。仅在氧气中执行反应过程.选择氧气流的值以确保氧气与蒸发的金属原子比率为约4∶5，以产生IF-2(经氧化的超级合金层)，其将导致涂层的几乎完全氧化.通过EDX测量非反应性过程A和反应性过程B之后的靶的化学组成，并和与原始粉末组成的差值(Δ)一起在表1中给出(第5至第8列).靶表面的分析表明Al和Cr从非反应性过程到反应性过程略微减少，但其它靶元素的组成没有急剧变化.在图2中给出在以非反应模式进行电弧操作之后的靶表面的XRD图(实线).与原始靶(虚线)相比，操作靶的峰更窄，并且朝向更高的角度移动。也可以将它们归为fcc立方相(Fm-3m)。操作靶的平均晶胞稍小，晶格参数从(操作前)降低到/>(操作后)，并且减小的半高宽(FWHM)表明靶表面上的再结晶过程。
涂层合成
通过非反应性处理，用表2中给出的方法A的参数合成涂层，以调查研究是否也可以在涂层中保持靶的化学组成。通过EDX获得的组成展示于表3中，在两种情况下，涂层A具有界面层(IF-1)的组成。除了C(EDX对C不够灵敏和精确)，分析表明仅Al浓度在涂层中降低并且Ti浓度在涂层中在某种程度上降低。对在SA-S基底上的涂层执行初始XRD分析。由于涂层和SA-S具有非常相似的晶格常数，因此所观察到的布拉格反射毫无疑义地归因于涂层。因此，针对蓝宝石基底上的涂层已进行重复测量(图7)。
两个观察到的相中的第一个，表示为M-1，其中(黑线，峰的左侧)，与未涂覆的SA-S相/>几乎相同(图7)。第二相M-2的反射(灰线，峰的右侧)朝向较高的2θ角移动/>这表明蓝宝石基底上的成核行为略有不同。相M-2的晶格常数已被确定为大约/>靶(和基底)材料的TEM调查研究已经表明超过一种金属间相，并且EDX图显示，除了一起偏析的沉淀物之外，还存在至少两组元素.有可能这两组在不同温度下冷凝，这导致这种相分离.
在额外的实验中，根据方法B调查研究了完整的叠层。在如上所描述的SA-S的初始预处理之后，通过电弧蒸发以非反应性模式形成IF-1，并且在SA-S处没有厚度为约500nm的额外的界面.在随后的步骤中，将800sccm的氧气送入电弧蒸发过程，并且执行从非反应性模式到反应性模式的短暂转变。连同基底的双旋转，这导致多层结构，并最终导致约1.5μm的氧化物涂层的成核。图8a中显示了完整叠层的STEM明场图像。在图8b和图8c中用虚线表示基底和界面层IF-1之间的界面。已通过图8c中的TKD和图8b中对应的图像质量图(在这里是黑白的)对界面进行更详细地调查研究。取向绘图显示IF-1区域中的晶粒处的外延生长，随后是具有任意取向的许多非常小的晶粒的成核，最后是较大晶粒的生长，即在该过渡区的较细晶粒处成核并形成叠层的氧化区.图9中给出了界面的放大区域的高分辨率(HR)-TEM显微照片.该显微照片证明，ST-A和涂层的晶格面平行，平面之间的距离相同，再次证实了涂层在基底上的外延生长。
因此，详细显示了通过以原位工艺顺序(即，不中断真空)进行的阴极电弧蒸发产生用于粘合涂层的完整叠层的可能性.已证明，可以由化学组成与超级合金基底几乎相同的粉末制造靶并在电弧蒸发中用作阴极.可以在非反应性和反应性沉积工艺中操作靶.对在有或没有氧反应性气体的情况下处理后的靶表面的调查研究揭示，对化学组成和晶体结构仅有极小的影响。以非反应性沉积模式合成的涂层在化学组成和晶体结构方面也与靶相似。在一种工艺中产生用于粘合涂层的完整叠层的方法，允许通过受控添加反应性氧气或通过操作具有相同或不同的元素组成的额外靶来进行梯度分布的设计原理.另外，在基底界面处的多晶基底的晶粒处可以观察到外延生长.向运行着的电弧蒸发过程中添加氧气导致细晶粒过渡区，并最终导致在叠层的完全氧化区中较大微晶的成核。所提出的方法具有在任意超级合金材料上实现外延生长和对具有不同化学组成和功能性的涂层执行渐变的潜力。表1
表2
表3
/>

Claims (7)

1.通过粉末冶金生产制造的超级合金靶，其中：
-所述超级合金靶具有随机晶粒取向的多晶结构和80-99％的fcc晶体结构，
-所述结构中的平均晶粒尺寸小于20μm，
-所述结构中的孔隙率小于10％，
-所述超级合金是以下合金之一：
以钴作为主要金属组分的钴基超级合金，其包含Cr、W、Ni、Al和Ir中的至少一种元素作为合金元素；或
-以镍作为主要金属组分的镍基超级合金，其包含Cr、Fe、Co、Mo、W、Al、Zr、Nb、Re、Y、V、B和Hf中的至少一种元素作为合金元素，
-所述靶由所述超级合金的合金粉末制备，并包含沉淀物，其为γ'和碳化物并且主要由Ta和Ti组成。
2.根据权利要求1所述的超级合金靶，其特征在于，就结晶学一致性和外延生长而言，所述超级合金靶主要具有同一种晶体结构，其中fcc晶体结构的比例在80％至99％的范围内。
3.根据权利要求1所述的超级合金靶，其特征在于，所述超级合金靶包含具有相似晶格常数的不同金属间相。
4.根据权利要求1-3之一所述的超级合金靶，其特征在于，原始靶的XRD图显示主峰，其被标示为fcc立方相，并且操作靶的XRD图显示与针对原始靶表面所观察到的fcc立方相类似的fcc立方相。
5.通过粉末冶金生产制造根据权利要求1-4之一所述的超级合金靶的方法，其中所述粉末冶金生产从超级合金的合金粉末开始，其中根据待涂覆的超级合金的组成来选择用于所述靶生产的粉末组成，其中在粉末的制造期间发生所述具有随机晶粒取向的多晶结构和80-99％的fcc晶体结构的超级合金靶的各相的合成，并且所述方法包括以下步骤：
-在1000-1350℃的温度范围内进行所述合金粉末的放电等离子体烧结而不牵涉液相的形成。
6.根据权利要求5所述的制造超级合金靶的方法，其特征在于，在真空下在两个石墨冲头之间的石墨模具中对粉末组合物加压并且同时施加DC电流或脉冲DC电流。
7.根据权利要求5-6之一所述的制造超级合金靶的方法，其特征在于，通过粉碎超级合金固体来制造所述合金粉末。
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