CN104995331B - 具有磨合层的dlc涂层 - Google Patents

具有磨合层的dlc涂层 Download PDF

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CN104995331B
CN104995331B CN201480009401.1A CN201480009401A CN104995331B CN 104995331 B CN104995331 B CN 104995331B CN 201480009401 A CN201480009401 A CN 201480009401A CN 104995331 B CN104995331 B CN 104995331B
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dlc
substrate bias
gradient
hardness
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CN104995331A (zh
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塞巴斯蒂恩·吉蒙德
曼弗雷德·乌尔泽
弗朗兹·威多维茨
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Oerlikon Surface Solutions AG Pfaeffikon
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    • 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
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    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/26—Deposition of carbon only
    • C—CHEMISTRY; METALLURGY
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    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/006—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterized by the colour of the layer
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/02—Pretreatment of the material to be coated
    • C23C16/0272—Deposition of sub-layers, e.g. to promote the adhesion of the main coating
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
    • C23C16/45523—Pulsed gas flow or change of composition over time
    • 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
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
    • C23C16/50—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating using electric discharges

Abstract

本发明涉及具有耐磨性的涂层，其中，首先在一个零件上施加具有高硬度的DLC层，并且在该DLC层上施加梯度层，该梯度层的厚度朝向表面减小。通过由此在梯度层中出现的硬度分布，该梯度层起到在利用滑动面的应用中的磨合层的作用。

Description

具有磨合层的DLC涂层
本发明涉及用于制造具有厚磨合层的耐磨层的方法。
背景技术
在具有滑动表面的构件中，对于硬质表面有着大量需求，但其作为外层具有磨合层，因而滑动的配对体首先能够至少部分磨损掉该磨合层，并因此达成匹配于其自身几何形状。
作为滑动层而已知的是：采用DLC层并且用比较柔软的层覆盖它，从而该比较柔软的层起到磨合层作用。但此时不利的是，必须转到另一层材料上。这对涂覆设备和要执行的涂覆方法提出更高的要求。
发明内容
因此，本发明任务是提供一种具有柔软磨合层的硬质表面涂层，其中，该硬质涂层和柔软磨合层的层材料基本相同，这涉及到化学元素及其浓度。
这是如此做到的，在DLC层上实现密度减小和进而硬度减小的梯度层。当梯度层足够厚时，由此产生有效的磨合层。
在此显然的是，因为梯度层较薄且密度减小，故这导致该层的总硬度减小。在一个优选实施方式中如此实现该梯度，即所述层的总硬度不小于15GPa。
根据本发明的另一个优选实施方式，该DLC层具有这样的硬度，该硬度不小于1500HV或15GPa，最好不小于18GPa，更好是不小于20GPa。
根据本发明的另一个优选实施方式，在梯度层厚度内没有硬度小于600HV或6GPa的区域，优选不小于8GPa。
根据本发明的另一个优选实施方式，DLC层的厚度不小于0.5μm。
根据本发明的另一个优选实施方式，梯度层的厚度不小于300nm。
根据本发明的涂层例如可以借助等离子体辅助CVD工艺、PVD工艺或者两者的组合来制造。
根据本发明的用于制造所述层的一个优选实施方式包括组合式等离子体辅助CVD和雾化工艺。
根据本发明的涂层尤其具有以下优点：
该DLC层保持足够坚硬以保证耐磨。
在具有较大粗糙度的基材上，甚至可以出现梯度层耐磨性的增大，因为在基材尖峰之间的区域得到了保护。
梯度层的制造可以基于用于DLC层制造的常规加工过程。不需要附加装备或附加气体。
附图说明
现在，将结合工艺描述来举例详述本发明。
图1与参照物相对照地示出了用于各种DLC样品的氢浓度。
图2示出了具有梯度的DLC样品与没有梯度的DLC样品的关于磨损的对照情况。
具体实施例
基材在真空室内借助等离子体辅助CVD方法来制造，在这里，采用了由乙炔和氩气构成的组合物作为工作气体。该工作气体在该室内借助等离子体被离子化，该等离子体是通过低压电弧放电产生的。还有，在涂覆工艺过程中施加“基材偏压(Substratbias)”于该基材。
为了DLC层的涂覆，基材偏压保持在900V的恒定值。DLC涂覆要求80分钟。为了涂覆梯度层，基材偏压连续从900V降低至50V。在经过了40分钟后，达到了50V的基材偏压。抛开基材偏压不算，在整个涂覆过程中，其它的涂覆参数保持不变。但是，低压电弧放电电流连续增大，以对抗伴随基材偏压降低而出现的基材电流减小。通过连续减小基材偏压，实现层密度的连续减小，这又导致了层硬度的减小。
结果，梯度层是0.7μm厚。用于整个体系(DLC层和梯度层)通过以10mN负荷微压印在涂层测厚仪(Fischerscope)上而测得的硬度等于18GPa。该层体系表现出优异的耐磨性。
氢原子浓度([H])的深度变化是利用2MeV He ERDA(弹性反冲探测分析)针对两个DLC样品来求出的：一个具有梯度，一个没有梯度。为了计算出数据，作为参照物测量具有9.5at％H的标准物(云母)，并且利用SRIM程序(www.srim.org)来确定在DLC层和标准物中的α粒子的能量损耗(减速能力)。无梯度的DLC层的涂覆是在900V的恒定基材偏压下进行的并且需要80分钟(层厚～1μm)。为了涂覆具有梯度的DLC层，基材偏压从900V连续地降低到50V。该步骤用时80分钟并且导致了1.5μm的梯度层厚。结果如图1所示。该方法允许测量直达约350nm深度。该表面在曲线图中靠右(0)，深度刻度向左移。结果表明，氢原子浓度朝着梯度表面增大。而在无梯度的DLC样品中，氢原子浓度保持不变。
带有梯度层的DLC的磨损利用针盘磨损试验(针盘摩擦计，CSM仪器)来试验，并且与DLC(无梯度层)比较。用于两次试验的基材是相同的(抛光钢盘)。试验在空气中在22℃温度和43％相对湿度下进行。样品相对直径为3毫米的100Cr6钢球进行研磨。钢球作为静态摩擦配对体，并且涂覆后的样品在钢球下旋转(半径6mm，速度30cm/s)。30N负荷被加到球上。在图2中，针对两个涂层示出了前50米和直到6000米后的代表性的摩擦系数。可以确定，具有梯度层的DLC的摩擦系数明显小于仅DLC的摩擦系数，尤其在初始阶段中。试验后的被摩擦的表面的检查也一般性地表明：“带有梯度层的DLC的层与配对体磨损”明显小于“仅DLC的层与配对体磨损”(涂层上的磨损印痕宽度是260μm对450μm，在球上的摩擦面的直径为300μm对600μm)。
利用在具体应用场合中的第一次现场试验，也能证明带有梯度层的DLC具有更好的磨合性能。

Claims (5)

1.一种在零件上的硬质材料层，其中，该硬质材料层包括其硬度至少为10GPa的DLC层，其特征是，在DLC层上设有至少300nm厚的DLC梯度层，
其中，该DLC梯度层以密度减小和进而硬度减小的方式实现，并且，
其中，该DLC梯度层与该DLC层相比全部化学元素没有差异。
2.根据权利要求1的硬质材料层，其特征是，该梯度层的化学成分只在氢含量上不同于该DLC层的化学成分。
3.一种制造耐磨表面的方法，其包括以下步骤：
-将待涂覆的基材装入涂覆腔；
-抽吸该涂覆腔，并且输入包含乙炔和氩气的工作气体；
-产生等离子体；
-将基材偏压施加到待涂覆的基材上；
其特征是，为了设置DLC层，首先施加高数值的基材偏压；并且为了随后涂覆DLC梯度层而减小该基材偏压，其中，以连续减小和/或以许多小的减小步骤来减小，
其中，抛开基材偏压不算，在整个涂覆过程中，其它的涂覆参数保持不变，以至于该DLC梯度层与该DLC层相比全部化学元素没有差异，且通过减小基材偏压，实现层密度的减小，这又导致了DLC梯度层硬度的减小。
4.根据权利要求3的方法，其特征是，在减小基材偏压的同时，连续增大低压电弧放电电流，以对抗随着基材偏压减小而出现的等离子体密度减小。
5.根据权利要求3的方法，其特征是，借助低压电弧放电产生等离子体。
CN201480009401.1A 2013-02-21 2014-02-10 具有磨合层的dlc涂层 Active CN104995331B (zh)

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Application Number Priority Date Filing Date Title
DE102013002911.2 2013-02-21
DE102013002911.2A DE102013002911A1 (de) 2013-02-21 2013-02-21 Dekorative, tiefschwarze Beschichtung
DE102013007146.1A DE102013007146A1 (de) 2013-04-25 2013-04-25 DLC Beschichtung mit Einlaufschicht
DE102013007146.1 2013-04-25
PCT/EP2014/000425 WO2014127902A1 (de) 2013-02-21 2014-02-10 Dlc beschichtung mit einlaufschicht

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