CN108884550B - 具有锆附着层的无氢碳涂层 - Google Patents

具有锆附着层的无氢碳涂层 Download PDF

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CN108884550B
CN108884550B CN201780018330.5A CN201780018330A CN108884550B CN 108884550 B CN108884550 B CN 108884550B CN 201780018330 A CN201780018330 A CN 201780018330A CN 108884550 B CN108884550 B CN 108884550B
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zirconium
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约格·韦特
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Abstract

本发明涉及带有硬质材料涂层的涂覆基材，硬质材料涂层包含硬的碳层和无氢无定形碳层，其中，该涂层包含在所述基材和无氢无定形碳层之间的由锆构成的层，并且其中，在所述由锆构成的层与无氢无定形碳层之间可以形成由Zr‑Cx构成的层，在由Zr‑Cx构成的层中形成碳化锆，并且其中，由Zr‑Cx构成的且包含碳化锆的层被直接施加到由锆构成的附着层。

Description

具有锆附着层的无氢碳涂层
技术领域
本发明涉及具有锆附着层的无氢碳涂层，用于基材表面、尤其用于针对摩擦学应用的工具表面或构件表面，其中，该碳涂层可能包含具有无氢无定形碳结构的硬碳层（视C-C sp3键含量而定，被称为a-C或ta-C）和其它元素，并且属于类金刚石（DLC）层系，并且该锆附着层由锆构成；其中，该锆附着层被如此施加在基材表面和硬碳层之间，即在碳层碳原子和锆层锆原子之间形成原子键。
在本发明的上下文中，“锆”是指元素符号为Zr的化学元素。
以下为简化起见，将Zr1-xCx简称为Zr-Cx。其中X表示原子百分比at%，且下列等式适用：0at%≤X≤50at%以及Zr(at%)+C(at%)=100at%，不考虑杂质。在X=0at%情况下，该附着层是纯锆层。但优选0at%≤X≤50at%的范围。
本发明意义上的碳层是指下述层，其具有可借助体积测量证明的无定形状态下的碳基体，其可以借助拉曼光谱法或其它合适的测量方法来证明。
该锆层用于在基材与无氢碳层之间“增附”。因加工过程原因，在无氢层碳原子和锆层原子之间形成原子键。在一定的加工过程条件下，根据加工温度和所出现的碳原子的“能”的不同，可能在由锆构成的层和无氢无定形碳层之间形成薄的Zr-Cx层。
还可以有目的地通过同时沉积碳和锆来形成一碳化锆，其中，由ZrC构成的层（或许含有一碳化锆的层）被直接施加到由锆形成的附着层。在另一个显现形式中，至纯碳层的过渡也可以是多层的或分级的无氢a-C:Zr层或ta-C:Zr层，其具有较大的碳原子相对于锆原子的原子百分比，而有别于化学计量的碳化锆。
背景技术
也称为DLC层的无定形碳基硬质材料层由现有技术公开了。但这种层并非总是充分附着于基材，尤其当它们是a-C类型或ta-C类型的无氢硬层时。这取决于所述层的高内部应力状态，由此难以沉积出具有出色功能性的工艺稳定地固着的这种类型层。
与此相关，Kabushiki例如在DE102007010595B4中教导了，当氮化物或碳氮化物被用于中间层时，由无定形碳(也称为DLC，其中DLC是英文“DIAMOND LIKE CARBON”的缩写)构成的层的附着甚至在高温时或者在高载荷范围内也可以被改善。因此，Kabushiki提出通过在基材和由无定形碳构成的DLC层之间沉积一个多层层系来产生在所述基材和由无定形碳(DLC)构成的层之间的附着。根据Kabushiki的教导，可以通过这种方式改善基材和DLC层之间的附着，即便是在高温下和在高载荷范围内。
根据Kabushiki的多层层系包含：
-形成在基材上的底层，其包含元素M的氮化物或碳氮化物并具有按照化学式M1-x- yCxNy的组成，在此，x≤0.5，y≥0.03并且1-x-y大于0，其中，M是选自元素周期表4A族、5A族和6A族、Al和Si中的至少一种元素，其中，元素M包含Ti、Zr、V、Nb、Ta、Cr、Mo、W、Al和Si，并且M优选包含元素W、Mo和Ta，以及
-形成在底层上的梯度层，其包含M、氮和碳，其中，从底层到位于梯度层上的无定形碳层，元素M和氮的含量减小，而碳含量增大，以及
-形成在梯度层上的表面层，其包含无定形碳层，无定形碳层由碳构成或者由至少50at%的碳以及由元素M构成的余量构成，并且可选地还有
-在基材和底层之间形成的下述元素的层，该元素可以从元素周期表中的4A族元素、5A族元素、6A族元素、Al和Si中选择。
但上述层结构是复杂的且因此需要复杂的反应涂覆方法，这大多在工业生产中如大批量生产中是不希望有的，因为工艺步骤的复杂性对足够高的涂覆产能而言是较高的危险。
发明内容
本发明的任务是提供硬质材料涂层，其包含硬的无氢无定形碳基层，其中，该硬质材料涂层具有尽可能简单的层结构和很好的与基材的附着，即便是应用在高载荷的区域中。
本发明的另一任务是提供一种涂覆方法，其容许以简单的方式但以更高的工艺稳定性制造涂层。
根据本发明的任务解决方案
根据本发明通过提供一种碳涂层来完成所述任务，该涂层包含硬的碳层和锆附着层，并且其中，该碳层具有坚硬的无氢无定形碳结构，该锆附着层由锆构成；该锆附着层施加在所述基材表面和所述硬的碳层之间；并且在所述锆附着层和所述硬的碳层之间形成Zr-Cx层，该Zr-Cx层包含一碳化锆并且包含在该硬的碳层的碳原子与该锆附着层的锆原子之间的原子键并且具有在5至500纳米之间的层厚；其中，该无氢无定形碳层为多层结构，该多层结构由a-C/Zr交替、ta-C/Zr交替、a-C/a-C:Zr交替、ta-C/ta-C:Zr交替、ta-C/a-C:Zr交替或a-C/ta-C:Zr交替。
该碳涂层包含硬的碳层和锆附着层；其中，该碳层具有硬的无氢无定形碳结构，该锆附着层由锆构成；且该锆附着层如此施加在所述基材表面和硬的碳层之间，即，由工艺决定地在硬的碳层的碳原子与锆附着层的锆原子之间形成原子键，在这种情况下，形成含有锆和碳的Zr-Cx薄层，其层厚为几个原子层或多达几纳米。
附图说明
图1a)示出在具有铬附着层的碳涂层上的洛氏硬度C（HRC）压痕的照片，
图1b)示出在根据本发明的碳涂层上的洛氏硬度C（HRC）压痕的照片，
图2示出根据本发明的带有支承层的碳涂层。
具体实施方式
在根据本发明的碳涂层的第一实施方式中，Zr-Cx层只通过由工艺决定地形成的、在硬的无氢无定形碳层的碳原子和锆附着层的锆原子之间的原子键来形成，使得该Zr-Cx层的层厚在原子层范围内。Zr-Cx层的层厚在此实施方式中例如可以是2~10个原子层。
在根据本发明的碳涂层的另一个实施方式中如此选择工艺条件，即在锆附着层沉积之后，尤其是工艺温度和撞击锆附着层表面的碳原子的能量促成在硬的无氢无定形碳层的碳原子和锆附着层的锆原子之间的原子键的形成，从而通过这种方式得到形成层厚为至少两个原子层到约100纳米的Zr-Cx层所需要的条件。
在根据本发明的碳涂层的又一个实施方式中如此进行加工处理，即在锆附着层和硬的无氢无定形碳层之间形成一个ZrCx层，其含有一碳化锆。含有一碳化锆的ZrC层可以通过同时沉积锆和碳形成。含一碳化锆的ZrCx层的层厚例如在此实施方式中为5至500纳米。
根据本发明的一个优选实施方式，无氢无定形碳层是a-C层或ta-C层。
被本领域技术人员称为a-C层或ta-C层的无氢碳层例如可以借助电弧法(未过滤或过滤)或也借助溅射法(DC、脉冲DC、RF或HiPIMS)被沉积，优选在a-C层情况下。
C-C键中的sp3键含量的相对占比等于或小于C-C键中的sp2键含量的占比之时使用术语“a-C层”来描述。所述层于是具有低于50GPa的硬度。如果sp3键含量的占比超出sp2键含量的占比，则是指ta-C层(四面体无氢无定形碳层)，其一般具有高于50GPa的硬度。显然，本领域技术人员可以采用已知的薄层硬度测量方法。
锆附着层可以例如借助电弧法(未过滤或过滤)或也通过溅射法(DC、脉冲DC、RF或HiPIMS)来沉积。
基于被加速的且一般从非100%电离化金属蒸气中提取出的金属离子(这样的金属离子净化方法大多具有500至1500伏的施加的偏电压)、在这里是锆的离子净化方法的特点是，这种工艺参数是可选的，从而形成在几纳米至几十纳米的厚度范围内的薄锆层，其形成该锆附着层。
根据本发明的碳涂层可用于涂覆由例如钢、硬金属、铝合金、铜合金、陶瓷材料、金属陶瓷或其它金属合金构成的基材。因为用于制造本发明碳涂层的涂覆温度低至100℃，故可以涂覆就基材材料或其它性能而言对温度极为敏感的基材。
尤其是例如可以涂覆切削刀具和成型模具。
构件部分例如阀件、叶片泵或汽车部件例如活塞销、活塞环、牵引杆、杯形挺杆或家用器具例如切刀、剪子、刀片或医用技术装置部件例如植入体和外科手术器具或其它装饰性物件例如表壳尤其也可以被涂覆上根据本发明的碳涂层。
作为用于沉积锆层的蒸镀源，不仅可以采用带有过滤器的电弧源，也可以采用不带过滤器的电弧源。同样，合适的锆层可以借助溅射法例如RF、DC、脉冲DC或HiPIMS来沉积。气相沉积例如电子束气相沉积、低压电弧蒸发或空心阴极电弧蒸发也适合沉积用于本发明的碳涂层的锆附着层。
除了a-C层和ta-C层外，也可以有目的地形成a-C:Me层或者ta-C:Me层。这些层包含至少一种金属作为掺杂元素，并且相比于没有掺杂元素的a-C层和ta-C层具有变化的性能曲线，例如导电性能更高。这因此可能在某些应用场合中是有利的。因为根据本发明的附着层应该由锆构成，故根据工艺有利地采用锆作为Me。
在借助电弧运行碳蒸镀的同时还进行锆蒸发的情况下，得到最简单的工艺过程控制。另一种方法是采用混有锆的碳靶。
本发明的另一个实施方式是无氢无定形a-C:X层或者ta-C:X层。
除了被加入所述层中且因此导致a-C:Me层的金属元素(统称为Me)外，也可以加入其它的非金属元素(总体用X标示)作为掺杂元素以便根据应用来优化层。非金属元素可以是氮、硼、硅、氟或其它元素。例如掺杂N或Si导致应力降低，掺杂F导致润湿性能变化(较大润湿角)，如本领域技术人众所周知的那样。
根据本发明的又一个优选实施方式，无氢无定形层被设计成多层的膜层，其中，该多层的层结构包含交替布置的A类型单层和B类型单层，其中，A类型单层由a-C或ta-C构成，B类型单层由Me或a-C:Me或ta-C:Me构成。与此相关地，例如可以如此采用锆作为Me，即形成a-C/Zr或ta-C/Zr或a-C/a-C:Zr或ta-C/ta-C:Zr类型的、还有其它组合形式如ta-C/a-C:Zr或a-C/ta-C:Zr的多层的膜层。
利用该方法可以制造较厚的层，这是因为这些层内的总内部应力得以降低。例如从金属层沉积阶段起进行与在实施例中一样的加工过程，层厚被限制到约500纳米，然后相同的加工过程进行多次如6次，从而除了锆附着层外，还出现其它五个中间层以及出现大于3μm的总层厚。这导致了较高的承载能力和耐磨性。
根据本发明的另一个优选实施方式，该无氢无定形层被设计成多层的膜层；其中，该多层的层结构包含交替设置的A类型单层和B类型单层；其中，该A类型单层由a-C或ta-C构成，该B类型单层由a-C:X或ta-C:X构成。与此相关地可以采用例如硅或氮作为X。
人们可以采用附加的电弧蒸镀装置来沉积这种层，其蒸发与X元素形成合金的石墨阴极；或者也可以采用其它合适的PVD方法如用以溅射X元素的溅射法。
A类型单层的厚度优选为不大于2000纳米且不小于5纳米。B类型单层的层厚也优选不大于2000纳米且不小于5纳米。
在此实施方式中也有利的是，可以将更大的层厚同时与在同一涂层中的优化应力状况相结合。
根据本发明的另一个实施方式，该锆层借助金属离子净化方法被施加到待涂覆基材上。
在借助未过滤电弧中的锆离子的金属离子轰击情况下，当在基材上采用例如-700伏或低于-700伏的偏电压时，同时出现薄锆层的生长。它于是可以用作本发明的锆附着层。在此情况下力求获得五纳米至几十纳米的层厚。
根据本发明的另一个优选实施方式，无氢无定形层作为由纳米复合材料构成的层而存在，该纳米复合材料包含基体材料和嵌入基体材料中的材料，其中该基体材料优选由a-C或ta-C构成，嵌入材料由尺寸在纳米级范围内的金属碳化物构成，例如在金属掺杂无定形碳层情况下，根据金属的不同由例如碳化钨(WC)或碳化铬(Cr23C6、Cr3C2)或者其它金属元素碳化物、优选碳化锆(ZrC)构成。
根据本发明的硬质材料层也可以包含在基材与锆附着层（无氢无定形碳层沉积于其上）之间的支承层，如图2所示。示出了基材205，基材上首先设有支承层207，随后是Zr-Cx层209，接着是无氢无定形碳层。该支承层提高表面机械承载能力。它优选由韧性高于无氢无定形碳层的材料构成。例如该支承层可以由ZrN构成。另外的氮化物(例如CrN、AlTiN)、碳氮化物(例如TiCN、ZrNC)或者碳化物(例如TiC、CrC)或者氮氧化物(例如CrNO)可以用作用于a-C层或ta-C层的支承层。所述层优选借助电弧或溅射来沉积。
根据本发明的硬质材料层也可以被如此沉积，即其在基材和由锆构成的附着层之间包含一个或多个另外的金属附着层。例如所述另一个金属附着层可以是借助采用铬离子的金属离子净化来制造的铬附着层，随后将锆附着层沉积在该铬附着层上。
根据本发明的硬质材料层也可以根据本发明借助HiPIMS技术来制成。例如无氢无定形层和/或支承层和/或锆附着层和/或所述一个或多个中间层可以借助HiPIMS方法被沉积。
根据一个变型实施方式，借助HiPIMS仅沉积所述a-C层。
根据另一个变型实施方式，锆附着层和a-C层两者都利用HiPIMS被沉积。
在这些变型实施方式中，形成很光滑的a-C层是有利的。
根据本发明的硬质材料层也可以根据本发明借助融合了HiPIMS技术和电弧技术的混合技术来制造。
例如所述无氢无定形层和/或支承层可以借助混合的电弧/HiPIMS方法来沉积，并且锆附着层借助采用锆离子的金属离子净化方法，基于HiPIMS工艺来沉积。此外，也可以直接用HiPIMS方法进行较厚的锆附着层的沉积。
例如所述无氢无定形层也可以借助混合电弧法来沉积，而支承层借助HiPIMS或混合电弧/HiPIMS方法来沉积，而锆附着层借助采用锆离子的金属离子净化法来沉积。
所述方法融合应该被视为用于制造本发明的硬质材料涂层的本发明方法的例子，而不是限制用于制造本发明的硬质材料层的可能方法。
根据本发明的以锆附着层来实现的涂层与对应于现有技术的带有铬附着层的涂层之间的对比：
a-C层(约40GPa硬度)和ta-C层(约55GPa硬度)的层沉积已在配备有电弧蒸镀装置的商用涂覆设备中实现。
有两个涂层批次，分别按照6种不同的工艺，根据具体工艺的不同，就所有工艺步骤而言执行相同的参数组。根据涂层批次的不同，不同的附着层被沉积到具有60HRC洛氏硬度的钢制试样体。在对应于现有技术的涂覆批次中，碳层沉积之前借助电弧蒸镀将铬附着层施加在试样体上，但在本发明的涂层批次中，锆附着层借助电弧蒸镀被施加。在锆附着层情况下，也借助机械滴滤进行沉积，或是以前置的挡牌或借助遮光帘结构（Jalousinenanordnung）。
如本领域技术所已知地，涂覆步骤首先是抽空至高度真空(0.001Pa)，接着执行加热步骤，小心维持约150℃的最高基材温度。接着进行借助电弧增强辉光放电（AEGD）方法的离子净化，随后使用铬或锆引燃电弧蒸镀装置的电弧以沉积约120+/-40纳米的金属附着层。为此加入相应的间歇期，以便不超出约150℃最大温度。在沉积纯碳层的过渡阶段中，使用合适的石墨阴极引燃电弧蒸镀装置的电弧，并且至少500伏的电压被加至基材，从而出现金属中间层的C离子轰击。接着调节出各不同参数以制造a-C层和ta-C层；为达此目的，选择就偏电压梯度而言的至纯涂层相的不同过渡，即将所加基材电压降低至较低值，一般不到100伏；以及选择不同的间歇期时间，用于调节最高涂覆温度和涂覆期间的不同基材电压。约1μm层厚被沉积到试样体。通过适当地组合有效涂覆温度和所加的负偏压可以在所述层中调节出各种硬度，该工艺领域是本领域技术人员已知的(在温度相同时，相比于偏电压较低的情况，采用达到100伏的较高偏电压提供了更高的硬度；相反，更高涂覆温度在恒定偏电压下造成较低硬度)。就铬附着层和锆附着层的参数而言的六种不同涂覆工艺的结果在纳米硬度方面以及在HRC压痕质量方面被评估。具有铬附着层和具有锆附着层的无氢无定形碳层都表现出相同的层硬度。
出乎意料地，尽管工艺过程相同，但在分别采用铬电弧蒸镀装置和锆电弧蒸镀装置的全部大量重复实验中表明了，根据本发明的包含锆附着层的碳涂层的附着强度比根据现有技术的包含铬附着层的碳涂层大许多。两种涂层的根据洛氏硬度C方法(HRC方法)的附着等级被测量并且在图1中示例性示出。图1a)示出了在带有铬附着层的碳涂层上洛氏硬度C压痕的照片，而图1b)示出了在相同加工条件下，在约60HRC硬度钢构件上的带有本发明锆附着层的碳涂层上的洛氏硬度C压痕的照片。与工艺过程控制和在涂覆室内的位置无关地，锆附着层提供了出色的HF1至HF2的附着等级，而在铬附着层情况下附着等级为HF2至HF4。
借助HRC方法所确定的、在本发明的带有锆附着层的涂层情况下更佳附着可靠性的一种可能解释可以是：碳层沉积到铬附着层上可能导致多种碳化物的形成，因此可能形成脆性Cr-C相。截然相反，在利用本发明的锆附着层时没有形成较脆的相，而是形成“塑性”相，其在某些情况下可包含一碳化锆(ZrC)。
因此，离子净化方法是指所有的刻蚀方法，其通过至少一种惰性工艺气体(例如氦、氖或氩)和/或金属的离子化，并使其向基材表面加速而获得在所述表面的溅射或注入效果。当离子净化方法主要用来除去杂质比如自然氧化物或者有机杂质时，只用惰性气体离子来工作通常就够了。所述加工过程还有所谓的电弧增强辉光放电(AEGD)法是本领域技术人员所已知的。此时如果以足够高的强度(例如可以通过偏电压大小来调节)和/或持续时间来进行离子净化方法，则从基材表面轰击出足够多的原子，以便在离子净化方法之后发生的金属离子净化方法或涂覆时获得良好的层附着。
类似于本申请的、除了工艺气体外还采用或者也仅采用金属离子的离子净化方法，金属离子净化方法(或也称为金属离子刻蚀)是指另一种刻蚀方法。在金属离子净化方法中使用例如由铬或锆构成的一个或多个金属源，其作用是将离子化的金属加速至基材表面。首先根据所加偏电压的大小和加在金属源上的电流量，可以目的明确地调节所蒸发的(例如在电弧过程中)或所溅射的(例如在溅射过程或HiPIMS过程中)材料的能量和数量。这样，本领域技术人员可以在利用上述金属例子净化基材表面的同时在基材上借助金属离子轰击获得净沉积。在蒸发量恒定情况下，所加偏电压的大小主要决定了是否出现所用金属在基材上的材料涂覆。如果还采用更高的偏电压(从约700伏起)，则除了净化基材表面外甚至还将所用的金属离子注入基材表面，注入可以达到几十纳米深。但在工艺参数相同情况下，与材料相关地可以出现几十纳米的净沉积量。本领域技术人员充分了解该方法，因而本申请所述的实施例不应被理解为对本发明是限制性的。
在本发明的上下文中，无氢无定形碳层是指氢含量<5at%且优选<2at%的所有的碳层，其中，可能有的杂质未被考虑在内。但是，本领域技术人员知道用于确定本发明的层膜的化学组成合适的表征方法，比如弹性反冲检测分析(ERDA)、卢瑟福背散射(RBS)或者二次离子质谱(SIMS)。

Claims (10)

1.一种在基材表面上的碳涂层，其中，该涂层包含硬的碳层和锆附着层，并且其中，
该碳层具有坚硬的无氢无定形碳结构，该锆附着层由锆构成；
该锆附着层施加在所述基材表面和所述硬的碳层之间；并且
在所述锆附着层和所述硬的碳层之间形成Zr-Cx层，该Zr-Cx层包含一碳化锆并且包含在该硬的碳层的碳原子与该锆附着层的锆原子之间的原子键并且具有在5至500纳米之间的层厚；
其中，该无氢无定形碳结构为多层结构，该多层结构由a-C/Zr交替、ta-C/Zr交替、a-C/a-C:Zr交替、ta-C/ta-C:Zr交替、ta-C/a-C:Zr交替或a-C/ta-C:Zr交替。
2.根据权利要求1所述的碳涂层，其特征是，在所述基材与所述锆附着层之间沉积支承层。
3.根据权利要求2所述的碳涂层，其特征是，所述支承层由含有以下组中的至少一种元素的氮化物和/或碳化物和/或氧化物构成，该组由元素周期表的第三、第四、第五或第六族以及Al、Si、B构成。
4.根据权利要求2所述的碳涂层，其特征是，所述支承层由含有以下组中的至少一种元素的氮化物和/或碳化物和/或氧化物构成，该组由元素周期表的镧系元素族构成。
5.一种用于沉积根据前述权利要求之一所述的碳涂层的方法，其中，锆附着层施加在所述基材表面和无氢无定形碳结构之间，并且，在所述锆附着层和所述无氢无定形碳结构之间形成Zr-Cx层，其中，该无氢无定形碳结构借助电弧蒸镀法和/或溅射法来沉积，其特征是，同时地沉积Zr和C，使得Zr-Cx层含有一碳化锆；其中，该无氢无定形碳结构为多层结构，该多层结构由a-C/Zr交替、ta-C/Zr交替、a-C/a-C:Zr交替、ta-C/ta-C:Zr交替、ta-C/a-C:Zr交替或a-C/ta-C:Zr交替。
6.根据权利要求5所述的方法，其中，该无氢无定形碳结构借助过滤电弧蒸镀法来沉积。
7.根据权利要求5所述的方法，其中，该无氢无定形碳结构借助HiPIMS方法来沉积。
8.一种用于沉积根据权利要求1至4之一所述的碳涂层的方法，其特征是，该锆附着层借助过滤电弧蒸镀法和/或溅射法来沉积。
9.根据权利要求8所述的方法，其特征是，该锆附着层借助HiPIMS方法来沉积。
10.一种用于沉积根据权利要求1所述的碳涂层的方法，其特征是，在该Zr-Cx层中的一碳化锆通过同时沉积锆和碳到该锆附着层而形成。
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