CN104995287B - 用于具有摩擦负荷的高温应用的涂层 - Google Patents

用于具有摩擦负荷的高温应用的涂层 Download PDF

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CN104995287B
CN104995287B CN201380053325.XA CN201380053325A CN104995287B CN 104995287 B CN104995287 B CN 104995287B CN 201380053325 A CN201380053325 A CN 201380053325A CN 104995287 B CN104995287 B CN 104995287B
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CN104995287A (zh
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M·L·泽比施
J·拉姆
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Ou Ruikang Surface Solutions Inc
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Abstract

本发明涉及用于具有摩擦负荷的高温应用的涂层。该涂层包含多层片层体系和顶部‑润滑层，其中该顶部润滑层含有钼作为主要组分。

Description

用于具有摩擦负荷的高温应用的涂层
本发明涉及用于曝露在高温应用中的部件、构件和工具的磨损保护涂层。部件，构件和工具下面统称为基材。
发明目的
高温下的应用在机械、结构和化学稳定性方面对构件、部件和工具的表面功能提出了极端的要求。为了保证长期稳定的表面功能并由此确保工业过程生产效率，本发明提供了用于构件、活动部件和造型工具及切削工具的硬质材料层体系，这种硬质材料层体系以令人满意的方式改善了在不同的工业应用时因明显提高的热负荷(也就是说，高于400℃的温度，下面称为高温应用)而造成的部件和工具的磨损。这种高温稳定的硬质材料层体系的基本性质如下：1)足够的磨蚀-磨损保护，2)足够的粘附-磨损保护，3)足够的层粘附和4)足够的温度稳定性(相稳定性和耐氧化性)。
发明描述
根据本发明，提出了包含多层片层体系作为基底的涂层体系。在该多层片层体系上提供具有至少一个层片的顶部-润滑层体系。该顶部-润滑层体系对外隔绝该涂层体系。该顶部-润滑层体系含有钼作为主要成分，并且根据占优势的高温-摩擦接触和由此而产生的表面的机械和化学负荷可具有相匹配的构造(Archtechtur)/微结构以及相匹配的组成。
下面将给出优选的构造/微结构和组成的详细说明。简化地，在下文中也将顶部-润滑层体系称作顶部-润滑层。
图1示出根据本发明的涂层
图2示出根据本发明涂层的截面(纳米层片)
图3示出根据本发明涂层的截面(纳米层片)
该顶部-润滑层的构造能够通过i)单层结构，ii)双层结构，iii)多层结构或iv)纳米层压结构来表征，其中在ii-iv)的情况中，微结构或化学反应历程被该结构改变。但是，把微结构和/或组成分等级在i-iv)的所有情况中是可能的和合适的，以确保对于各自的应用而言与所需的机械性能协调一致的润滑性能。原则上，在所有情况中，所述层是纳米级性质的。该顶部-润滑层的化学组成通常如下表征：Moa-Xb-Yc，其中a、b和c给出各成份的原子浓度，且a+b+c＝1，钼被认为是主要成份，也就是说，0≤b＜a和0≤c＜a，其中X为可变的金属成份：B、Si、V、W、Zr、Cu和Ag或它们的组合，其中Y为可变的非金属成份：C、O和N或它们的组合。
特别优选地，在高于500度的高温应用下，顶部-润滑层具有下列组成：
Mo和/或Mo-Cu
Mo-N和或/Mo-Cu-N
Mo-O-N和/或Mo-Cu-O-N
Mo-Si-B和/或Mo-Si-B-N
Mo-Si-B-O-N
该顶部-润滑层优选包含至少95原子％的钼。该顶部-润滑层特别优选不含铝。该顶部-润滑层的层厚度优选在0.25-1.5微米之间，特别优选在0.5-1.0微米之间。
优选地，对于某一高温应用(温度、摩擦接触、环境气氛和时间长短)评定由顶部-润滑层和位于其下的层体系构成的合适的对。
在下文中意在说明例如Mo-X-Y顶部-润滑层与位于其下的多层片层体系的相互作用。考虑在不同的高温应用场合下的机械、结构和化学稳定性，顶部润滑层与位于其下的多层片层体系组合的作用机理也许能够描述如下：仅在摩擦接触的起始阶段通过在高温下连续耗尽该顶部-润滑层，形成固体润滑相(主要是金属氧化物)使用该顶部-润滑层，并由此优化摩擦磨合性能(也就是说调节进一步的进程的起始摩擦接触)，而位于其下的多层片层体系(在通过顶部-润滑层实现表面调节后)负责长时间和高温稳定地维持(磨蚀和粘附的)磨损保护。可认为，在自大约400℃起的温度下开始顶部-润滑层的氧化(取决于确切的微结构和组成)。含于顶部润滑层中的金属，如B、V、W、Zr、Cu、Ag和Mo的氧化能够导致形成所谓的″Magneli相″。众所周知，这种Magneli相具有极好的润滑性能(固体润滑)。相反，位于其下的多层片层体系由于其与该层层片化学反应历程协调一致的构造不仅提供了所需的机械、结构和化学的高温稳定性，而且在最高1000℃的高温下，在稳定的长期使用中提供了值得追求的和在这种情况中可控的固体润滑相(主要是金属氧化物；可导致形成所谓的″Magneli相″的形成。
根据本发明，该多层片层体系至少包括一个高温稳定化的层(HT-层)。这样的层例如可有相应于(Me1、Me2、Mo)N的组成。
在本发明的一个特别优选的实施方案中，该多层片层体系含有至少两个层组(Schichtpaket)，在该层组中随增加的基材间距在HT-层之后是润滑活性层。润滑活性层可相应于HT-层构成，但具有升高的钼比例。与此相应地，贫钼层形成了HT-层，而富钼层可形成润滑活性层。优选地，富钼层中的最大钼浓度超过相邻贫钼层的最小钼浓度至少10原子％，特别优选至少20原子％。交替层体系的富钼层例如可借助PVD-方法使用单组分材料源(靶)或借助PVD-方法使用多组分材料源沉积。
为了进一步改善润滑作用，交替层体系的富钼层能够包含由C、O、B、Si、V、W、Zr、Cu和Ag构成的组中的一种或多种其它的元素。
为了进一步改善高温稳定性，例如通过机械和化学性质的改善，交替层体系的贫钼层可包含由B、Si、Si、W和Zr构成的组中的一种或多种其它的元素和它们的混合物。
根据本发明，在该多层片层体系上布置上述的顶部-润滑层。
根据本发明的基材，也就是说用根据本发明的涂层体系涂覆过的基材可有利地在应用中产生高温和产生摩擦负荷的所有领域使用。例如，在直接加压淬火时，就是这样的情况。作为实例在此可提及：
○AlSi-涂覆的22MnB5USSH-片的直接加压淬火
○未涂覆的22MnB5USSH-片的直接加压淬火
其它的应用实例是
○高硬金属片的锻压
○特别是高硬钛-和镍合金的切削加工和成形
○内燃机中和涡轮压缩机领域中的构件和活动部件
○铝-和镁压铸
○特别是高硬塑料或铝的注塑和挤出
根据本发明的第一个实施例，在加压淬火模具上施加2微米厚的(Ti0.5Al0.5)N层。随后接着是5个层组，其中每个层组包含一个0.5微米厚的(Ti0.3Al0.3Mo0.4)N层，在其后是0.5微米厚的(Ti0.5Al0.5)N层。一个0.5微米厚的(Ti0.3Al0.3Mo0.4)N层构成该多层片层体系的终端。与此相反，整个层体系被作为顶部-润滑层的0.5微米厚的Mo0.95-Si0.03B0.02封闭。在该具体的情况中，作为合适的顶部-润滑层，MoN和Mo0.95Cu0.05N也具有特别重要的意义。
根据本发明的第二个实施例，在加压淬火模具上施加2微米厚的(Al0.65Cr0.25Si0.05)N层，其中Si任选地也能略去。随后接着是5个层组，其中每个层组包含一个0.5微米厚的(Al0.42Cr0.18Mo0.35Cu0.05)N层，在其后是0.5微米厚的(Al0.7Cr0.3)N层。一个0.5微米厚的(Al0.42Cr0.18Mo0.35Cu0.05)N层构成该多层片层体系的终端。与此相反，整个层体系被作为顶部-润滑层的0.5微米厚的MoN层封闭。
此外，优选具有一方面包含Al和B和IV和V副族元素的化合物(C和/或N和/或O)和另一方面包含Mo-化合物(C和/或B和/或N和/或O)的多层片层体系和具有顶部-润滑层的涂层，该顶部-润滑层包含具有Mo作为主要成分的Mo化合物并且其厚度等于大于、优选比多层中的含钼层的厚度厚。
具有上述多层片层体系的涂层是特别优选的，在该体系中在金属的总份额中钼的整体份额＜50原子％。
进一步的试验产生本发明的特别优选的实施方式的下列特征：
-润滑活性层(TiAlMoN)应该有利地具有20-60原子％，优选25-35原子％，特别优选30原子％的钼含量(平均值；在10千伏下用EDX测量时)。
-也可通过润滑活性层的构造(纳米层-结构)控制(平均)钼含量(见下图)。使用2靶-型号(Mo和TiAl)，技术上其可通过i)改变转动速度和/或通过ii)改变所有同时运行的靶的靶参数来实现。
-在TiAlMoN(纳米层中的浅色层)中富MoN层的厚度可以在10-60纳米之间，优选在20-50纳米之间，特别优选在30-40纳米之间变化。TiAlMoN中富MoN层的最佳厚度似乎在约40纳米处。
-润滑活性层(TiAlMoN)中约30原子％的Mo含量可在约800-900℃的温度下非常有利地推动表面氧化(未不利影响整个层结构)，由此始终提供足够的(氧化物)润滑剂，以阻止长期使用时AlSi润滑耗尽(Aufschmieren)。这已为接近应用的实验(例如用连续交替的Usibor-片的HT-SRV-实验，其中始终测试同一层)所证实。
下列的事实也是非常有利的，即在润滑层(TiAlMoN)中的Mo-含量在20-40原子％的范围变化的情况下，整个层的机械性质(硬度、E-模量、粘附)、结构性质(相组成)以及氧化性质(氧化物层在800℃在环境气氛中生长1小时)并未显著地改变。这使得有针对性地优化就耐磨蚀-和粘附-磨损而言的各种应用的构造和组成成为可能。

Claims (8)

1.具有多层片层体系和顶部-润滑层的涂层，其中所述多层片层体系包含至少一个HT-层，所述顶部-润滑层具有组成Moa-Xb-Yc，其中a、b和c给出各自成分的原子浓度，并且a+b+c＝1，0≤b﹤a和0≤c﹤a，其中X为可变的金属成分：B、Si、V、W、Zr，Cu和Ag或它们的组合，其中Y为可变的非金属成分：C、O和N或它们的组合，其中所述多层片层体系包含至少一个润滑活性层，其特征在于，所述至少一个润滑活性层是Ti-Al-Mo-N层，其具有用EDX在10千伏下测得的20-60原子％的平均Mo含量。
2.根据权利要求1的涂层，其特征在于，所述至少一个润滑活性层由富MoN的纳米层和贫MoN的纳米层构成。
3.根据权利要求2的涂层，其特征在于，所述富MoN的纳米层有10-60纳米。
4.根据权利要求1的涂层，其特征在于，所述Ti-Al-Mo-N层具有25-35原子％的平均Mo含量。
5.根据权利要求1的涂层，其特征在于，所述Ti-Al-Mo-N层具有30原子％的平均Mo含量。
6.根据权利要求2的涂层，其特征在于，所述富MoN的纳米层有20-50纳米。
7.根据权利要求2的涂层，其特征在于，所述富MoN的纳米层有30-40纳米。
8.根据权利要求2的涂层，其特征在于，所述富MoN的纳米层有40纳米。
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