CN109072407B - 特别是活塞环的滑动元件 - Google Patents

特别是活塞环的滑动元件 Download PDF

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CN109072407B
CN109072407B CN201780026888.8A CN201780026888A CN109072407B CN 109072407 B CN109072407 B CN 109072407B CN 201780026888 A CN201780026888 A CN 201780026888A CN 109072407 B CN109072407 B CN 109072407B
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马卡斯·肯尼迪
尤里·伊万诺夫
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Abstract

特别是活塞环的滑动元件具有涂层，该涂层从内向外具有以下层：多晶的、金属掺杂的粘结层、中间层和至少一个非晶碳层，中间层从内向外具有以下部分层：AxCy层，C代表碳，A代表优选金属掺杂粘结层的金属，x和y分别包含1‑99的值；以及含结晶或含晶体碳层。

Description

特别是活塞环的滑动元件
技术领域
本发明涉及滑动元件，特别涉及具有涂层的活塞环。
背景技术
对于暴露在部分地超过300℃的温度并且尽可能长时间具有最低的可能的摩擦系数的活塞环，众所周知地会设置含有粘结层、一个或多个DLC层以及可选地含有中间层的层系统。
DE 10 2008 042 896 A1教导了一种备选的方法，其公开了一种用于涂覆滑动元件的方法，特别是涂覆活塞环和内燃机汽缸衬套的方法，其中在硬质材料层的沉积过程中，DLC相嵌入在硬质材料层中。
可以在VDI指南2840中可以找到不同DLC层的类型及其属性的概述。例如，此处提供了最大热稳定性的下列值：
层类型 最大热稳定性
a-C 450℃
ta-C 500℃
a-C:H 400℃
ta-C:H 500℃
a-C:Me(Me＝W,Ti…) 400-600℃
a-C:H:Me(Me＝W,Ti…) 350-500℃
由此可知，DLC层系统的热稳定性和粘附性原则上可以通过高的sp3量、高的弹性模量和足够厚的粘合层来整体地保证。
热稳定性可以通过掺杂[Wu,W.-J.,Hon,M.-H.(1999).Surf.Coat.Technol.111:134–140.]、通过晶体结构[Zhang,S.,Bui,X.L.,Li,X.(2006)Diamond and RelatedMaterials 15:972–976.]，或通过生产工艺[Jung,H.-S.,Park,H.-H.,Pang,S.S.,Lee,S.Y.(1999)Thin Solid Films 355–356:151–156.]得到进一步改善。环境大气条件也是相关的[Ronkainen,H.,Likonen,J.,Koskinen,J.,Varjus,S.(1996).Surf.Coat.Technol.79:87–94.]。
在最初的发动机点火测试(fired engine test)中，发明人确定在柴油机应用中位于压缩环上的端部间隙区域中的ta-C涂层在运行100小时后已经脱落，因此活塞环在其密封性能方面的功能受到损害，但是，组件寿命也是如此(见图1)。从模拟中可以计算出，使用柴油机活塞，第一凹槽中的温度可以部分达到330度以上。因此，这些温度被认为是关键的，尽管它们远低于文献中规定的ta-C层热阻的最大值(根据VDI指南2840，最高达500℃)。
发明内容
本发明的目的在于提供一种滑动元件，该滑动元件尤其是在涂层的热和/或热化学粘附方面得到改进，特别是提供一种具有这种特性的活塞环。特别地，提供基于DLC涂层类型的层系统，在发动机应用中其极大地提高了热阻，使得层能够承受所提到的最大发动机温度并具有一致的耐磨性。
该目标通过权利要求书1中描述的滑动元件得到了解决。
根据其得知，它具有涂层，此涂层从内向外包括以下层：多晶的、金属掺杂的粘结层、中间层和至少一个非晶碳层。因此，中间层由内向外至少具有AxCy层和含结晶或含晶体或含微晶碳层，其中C代表碳，A代表优选为金属掺杂粘结层的金属，此外x以及y分别包含1-99的值。由此可以从VDI指南2840中提供的类型中选择非晶碳层的层类型。
本发明基于以下理解，粘结层是多晶的，而外层(由于始终如一地确保低摩擦系数的功能而被称为功能层)是非晶的。为了确保所有层的有利过渡和良好粘附，首先将中间层设置在粘结层上。前者具有相对薄、紧凑和定向、部分纹理化的含晶体结构，因此确保了稳定性，并且原则上，防止了该层内以及粘结层方向和功能层方向上的可能的扩散过程。利用所描述的层结构，能够在第一实验中确定改善耐热性和粘结性。涂覆优选通过所谓的PVD-Arc技术进行。
图2显示了根据本发明的涂层结构的图像并且表明即使在与图1所述相同的发动机中进行300小时的发动机运行后，获得了专利权利要求书1中描述的滑动元件的热稳定性。
在其他权利要求中描述了根据本发明的滑动元件的优选改进。
优选地，滑动元件在AxCy层和含结晶或含晶体碳层之间具有由混合相构成的过渡层，混合相为AxCy层和含结晶或含晶体碳层。这种层结构使得部分层之间的粘结性提高。
对于AxCy层(优选的也是粘结层)的金属A，例如提供了钛、钨、任何过渡金属并且尤其是铬。
此外，对于在粘结层中上述金属的氮化物和碳氮化物的预期结果是良好的。
此处还发现，粘结层应该具有大于80nm的厚度以便于在使用中充分地均衡因为机械或热引起的横向力，即实现滑动元件，特别是活塞环基底材料。
对于AxCy层的厚度，当前优选为3nm至10nm，优选4nm至8nm。
对于含结晶或含晶体碳层，已经发现厚度≤35nm是有利的。
过渡层的厚度优选为1至25nm，以便于实现所述的有利效果。
对于至少一个非晶碳层，优选它是无氢和/或未掺杂的(根据VDI指南2840，这意味着氢含量≤3At％)，因为这种层具有更高的耐磨性和更低的摩擦系数，特别是当用于内燃机时。
设置至少两个非晶碳层是特别优选的，进一步优选地，内部非晶碳层具有比外部非晶碳层更高的平均弹性模量。因此，在外部碳层内弹性模量可以连续降低，以协调整个C层内的残余应力。
特别地，在具有两个非晶碳层的系统中，已经证明E1＞300Gpa的平均弹性模量对内层是有利的，因为可以确保上述的紧凑性。
对于外部非晶碳层，目前优选的是平均弹性模量E2＜E1。这允许弹性地吸收剪切力，并且例如实现改善的磨合行为。此外，外部非晶碳层的弹性模量可以从内向外地减小。
对于内部非晶碳层，换句话说优选具有相对高的弹性模量的非晶碳层，目前优选其厚度是为总厚度的5％至30％。
对于总厚度，进一步证明1μm至50μm是有益的。
附图说明
图1显示了在柴油发动机中进行了100小时高功率发动机运行后，涂覆有传统ta-C的活塞环在端部间隙处的运行表面损坏。
图2显示了在柴油发动机中进行300小时发动机运行之后，根据本发明的涂覆有ta-C的活塞环的端部间隙的图像。
具体实施方式
特别地，目前优选的是从内向外具有铬粘结层、中间层(由CrxCy层、CrxCy层和含结晶或含晶体碳层的混合相过渡层以及含结晶或含晶体碳层组成)以及两个无氢非晶碳层的层结构，其中部分层具有权利要求5至8中限定的层厚度。
特别是与较薄的粘结层和较厚的含结晶或含晶体碳层相比，优选的结构能够确定在含氧气氛中高达50度以上的热稳定性。具体地，比较的例子中的粘结层具有＜80nm的厚度，并且含结晶或含晶体碳层具有40nm至60nm的厚度。
有利地将PVD-Arc方法用作生产方法。
例如，C离子可以以高能量穿透粘结层来产生仅仅几纳米厚的CrxCy层。出于能量原因，C离子不仅穿透该层，而且还存在离子再次扩散到表面并由此形成第一含结晶或含晶体碳层的可能性。该效应被称为亚注入，并在J.Robertson的论文中详细描述(J.Robertson,Diamond-like amorphous carbon；Material Science and EngineeringR37；2002；129-281)。
该层由高能C离子引起，在本文中称为含结晶或含晶体或含微晶碳层。该层可以是半结晶的(nc-石墨，即形成单独的随机取向的簇)或结晶的(定向的类簇级)，其中碳原子主要是sp2杂化的。因此，CrxCy层的类簇级的最大膨胀或延伸约为100nm。类簇级之间的距离可以非常小至原子水平。此外，该层中包含的结晶C相在纳米级上。根据A.C.Ferrari和J.Robertson(Physical Review B；Vol 61；Number 20；2000；14095-14107)，所谓的拉曼光谱可以检测到工艺参数带来的变化。根据本发明的的涂层(特别是中间层)的例如通过TEM和SAED(“选区电子衍射”)的电子显微镜研究显示了衍射图像中对应于图形反射(Graphen-Reflexen)的半椭圆反射。由此可以推断出在中间层碳层中的结晶碳以及其部分结晶度的存在。在TEM中，可以看到中间层离散圆的明亮场图片以及椭圆图形反射，该离散圆表明了Cr的立方空间中心晶格。这进一步揭示了根据本发明的滑动元件的涂层的中间层或过渡层中结晶Cr相和结晶C相的共存。
已经发现在后续由具有较低能量的C离子沉积产生非晶碳层的过程中，如果在粘结层和非晶碳层之间设置本发明的中间层，那么就可以确保优异的粘结性。特别是，如果含结晶或含晶体碳层太厚，则不再能吸收横向力，因为含结晶或含晶体碳层的晶面以优选的角度生长至表面。然后将非晶功能C层与含结晶或含晶体碳层分离。横向力可以由外部机械力引起，例如，通过在混合或限制摩擦条件下连接的内燃机气缸中的活塞环的上下运动或通过热能，这导致由显著不同的热膨胀系数在过度铁基基底到碳层中产生应力。
通过关于这里提到的关于层的实验，通过C离子的强加速实现了Cr和C混合成CrxCy以及CrxCy和含结晶或含晶体的碳层的混合物。通过高的所谓BIAS电压实施加速，该电压直接在元件处调节。太高的温度导致形成C簇，主要具有sp2键的C簇，优选各向异性分布的C簇，通过该簇，过渡的稳定性降低。在小于120℃下，形成更加各向同性的富含sp2的晶面，即所谓的nc石墨。它们具有高的热稳定性和机械稳定性。
因此，对于中间层，优选保持30至120℃的温度和500至1200V的BIAS电压，同时对于DLC功能层，优选调节小于250℃的温度和10至200V的BIAS电压。如本领域技术人员所知，通过在上述参数范围内调节电压和温度，特别是也能够调节根据本发明的弹性模量曲线。
以上对于基于Cr的实施例示例的就中间层和过渡层的性质和(纳米)结构所做的所有陈述特别适用于本发明包含的所有涂层。

Claims (19)

1.滑动元件，所述滑动元件具有涂层，所述涂层从内向外具有以下层：
-多晶的、金属掺杂的粘结层，
-中间层，以及
-至少一个非晶碳层，
所述中间层从内向外至少具有以下部分层：
-AxCy层，C代表碳，A代表优选为金属掺杂粘结层的金属，x和y分别包含1-99的值，以及
-含结晶碳层，其中，碳原子主要是sp2杂化的。
2.根据权利要求1所述的滑动元件，
其特征在于，
所述滑动元件在所述AxCy层和所述含结晶碳层之间具有过渡层，所述过渡层由所述AxCy层和所述含结晶碳层的混合相构成。
3.根据权利要求1或2所述的滑动元件，
其特征在于，
金属A选自钨、钛、铬或其他过渡金属。
4.根据权利要求1或2所述的滑动元件，
其特征在于，
所述粘结层含有金属的氮化物或碳氮化物。
5.根据权利要求1或2所述的滑动元件，
其特征在于，
所述粘结层的厚度大于80nm。
6.根据权利要求1或2所述的滑动元件，
其特征在于，
所述AxCy层的厚度为3nm至10nm。
7.根据权利要求1或2所述的滑动元件，
其特征在于，
所述含结晶碳层的厚度不大于35nm。
8.根据权利要求2所述的滑动元件，
其特征在于，
所述过渡层的厚度为1nm至25nm。
9.根据权利要求1或2所述的滑动元件，
其特征在于，
至少一个非晶碳层是无氢和/或未掺杂的。
10.根据权利要求1或2所述的滑动元件，
其特征在于，
具有至少两个非晶碳层。
11.根据权利要求10所述的滑动元件，
其特征在于，
内部非晶碳层具有比外部非晶碳层更高的弹性模量。
12.根据权利要求10所述的滑动元件，
其特征在于，
内部非晶碳层的平均弹性模量大于300Gpa。
13.根据权利要求10所述的滑动元件，
其特征在于，
外部非晶碳层的平均弹性模量小于内部非晶碳层的弹性模量。
14.根据权利要求10所述的滑动元件，
其特征在于，
外部非晶碳层的弹性模量沿表面方向从内部碳层开始减小。
15.根据权利要求10所述的滑动元件，
其特征在于，
内部非晶碳层占总厚度的5％至30％。
16.根据权利要求1或2所述的滑动元件，
其特征在于，
总厚度为1μm至50μm。
17.根据权利要求1或2所述的滑动元件，
其特征在于，
利用PVD方法生产层。
18.根据权利要求1所述的滑动元件，其特征在于，所述滑动元件为活塞环。
19.根据权利要求6所述的滑动元件，其特征在于，所述AxCy层的厚度为4nm至8nm。
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