CN112424466B - 用于涂覆至少一个金属构件的方法 - Google Patents
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Abstract
本发明涉及一种方法,适用于涂覆至少一个金属构件、尤其是喷射嘴的至少一个喷嘴体,其中,所述方法(100)在具有HiPIMS组件和通过ECR等离子体源运行的等离子体浸没植入组件的过程腔中运行,所述方法具有下列方法步骤:a)将所述至少一个构件作为三维衬底引入(110)到所述真空腔中,b)根据当前要构造的层类型选择(120)所述组件中的一个组件,c)激活(130)所选择的组件,以便构造具有预先确定的层厚度的层,并且d)必要时重复方法步骤b)至c),直至在所述构件上分别构造不同层类型的层。
Description
技术领域
本发明涉及一种用于涂覆至少一个金属构件、尤其是至少一个喷射嘴的方法,并且涉及一种根据这种方法涂覆的构件以及尤其适用于实施这种方法的设备。
背景技术
为了抵抗例如会损害构件的功能优越性和/或限制所述构件的使用寿命的磨损效应,通常将承受特别强烈的负荷的构件涂覆防磨损层。尤其在作为燃料喷射嘴的部件的喷嘴体中出现以下问题:尤其地,装入喷嘴体中的喷射孔(所述喷射孔的尺寸影响燃料喷射嘴的喷射行为)的内面通过传统的涂覆方法、如CVD(“chemical vapor deposition”化学气相沉积)或ALD(“atomic layer deposition”原子层沉积)几乎不能被令人满意地涂覆,因为一方面在CVD中所需要的高过程温度以化学的方式剧烈地减少所基于的衬底材料并且另一方面通过ALD方法决定地不能沉积足够厚的层。虽然可以在相对低的过程温度中制造所谓的DLC层(“diamond-like coating”类金刚石涂层)作为防磨损层,但通常为了沉积所述DLC层所使用的方法、如PVD(“physical vapor deposition”物理气相沉积)和PECVD(“plasmaenhanced chemical vapor deposition”等离子体增强化学气相沉积)不那么适用于涂覆喷射孔的孔内面。因此,例如由基本上致力于沉积在硅衬底上的DLC层的基于等离子体的离子植入的S.Miyagawa等人的研究示出,在弯曲的钢管上借助基于等离子体的离子植入沉积的DLC层具有不均匀的层厚度变化曲线,其中,在管内面上的层厚度还构造地明显低于在外面上的层厚度(S.Miyagawa等人:“Deposition of diamond-like carbon films usingplasma based ion implantation with bipolar pulses”,Surface and CoatingsTechnology 156(2002年)第322至327页)。S.Peter等人的研究公开了,非晶含氢碳层(a-C:H)和非晶含氢碳氮化硅层(SiCN:H)借助于不同的等离子体诱导的CVD沉积方法在平面的硅晶片上、即在半导体衬底上的沉积(参见S.Peter等人:“Low temperature plasmaenhanced chemical vapor deposition of thin films combining mechanicalstiffness,electrical insulation,and homogeneity in microcavities”,Journal ofApplied Physics 108,043303(2010年))。
发明内容
具有权利要求1的特征的方法具有以下优点:作为具有大部分非平面的结构的三维衬底的构件能够可靠地涂覆有功能层或防磨损层和/或金属粘附层,其方式是,根据层类型将所述构件浸入到等离子体中,该等离子体在由固体相沉积的情况下借助于HiPIMS(大功率脉冲磁控溅射:“high power impulse magnetron sputtering”)产生或者在由气相沉积的情况下借助脉冲运行的等离子体浸没植入产生,该等离子体浸没植入通过ECR(Elektron-Zyklotronresonanz,电子回旋共振)等离子体源运行。尤其地,由此不仅能够涂覆喷射器喷射嘴体的外面,而且也能够涂覆所述射器喷射嘴体的典型地以亚毫米数量级构造的喷射孔的内面,因为一方面通过这两个等离子体产生类型可以分别产生高等离子体密度,并且另一方面电荷载体通过具有在微秒范围内的高压脉冲的短暂脉冲运行从等离子体区出发以高速度在脉冲周期中冲击式地转向或加速至要处理的构件,在那里植入并且由此引起一定厚度的层构造,通过该层构造可以实现高的和充分的防磨损。为此,根据本发明的方法在具有HiPIMS组件和通过ECR等离子体源在脉冲操作模式中运行的等离子体浸没植入组件的过程腔中运行,所述方法包括方法步骤:a)将至少一个构件作为三维衬底引入到真空腔中,b)根据当前要构造的层类型选择所述组件中的一个组件,c)激活所选择的组件,以便构造预先确定的层厚度的层,并且d)必要时重复方法步骤b)至c),直至在所述构件上分别构造不同层类型的层。
本发明的另外的有利扩展方案和构型由在从属权利要求中列举的措施得出。
符合目的地,在选择和/或激活等离子体浸没植入组件时将至少一种用作为前体的气体或气体混合物以掺杂的方式导入到真空腔中。在此,气体颗粒达到由ECR等离子体源产生的等离子云中,在那里离子化并且作为离子导向至所述构件。当要沉积构造为非晶含氢碳层的功能层时,这种前体可以是碳氢化合物、如乙炔。
根据本发明的方法的特别有利的构型设置为,所述至少一个构件在方法步骤c)期间通过对应于所选择和激活的组件的脉冲发生器的高压脉冲在没有对应于所述构件的衬底支架的中间电连接的情况下受到电加载。由此可能的是,仅仅要涂覆的构件通过在微秒范围内脉冲的高压加载,而对应的衬底支架可以保持在明显更低的电位上,由此可以减小电流负载。
为了尽可能避免在相应运行的沉积过程中的层次效应(Abschattungseffekt)并且在衬底的孔结构中也实现尽可能均匀的涂覆,符合目的的是,所述至少一个构件在方法步骤c)期间在真空腔中至少暂时地运动和/或所述至少一个构件在方法步骤c)期间围绕至少一个旋转轴线至少暂时地旋转。
包括这种方法的批量方法由于尽可能自动化的流程适用于涂覆较大件数的构件。
按照这种方法涂覆的构件有利地具有均匀的和持久的涂层。
尤其用于实施根据本发明的方法的设备设置为,构造为真空腔的过程腔具有HiPIMS组件和通过ECR等离子体源在脉冲操作模式中运行的等离子体浸没植入组件,并且与两个组件共同作用的控制和协调装置设置成用于根据当前要构造的层类型选择、激活并且控制这两个组件中的一个组件。由此,构件能够在单个设备或设施中连续地涂覆有不同层类型的层。
本发明的扩展方案可以在于,控制和协调装置在所选择的组件中使与该组件相对应的脉冲发生器在高压输出侧与所述至少一个构件电连接。控制和协调装置使相应脉冲发生器的高压脉冲不与衬底支架电耦合,而是替代地在所选择的脉冲发生器的高压输出部和所述至少一个构件之间引起电连接,由此能够保持限制所述设备的本身高的电流需求。
包括这种设备的批量设施由于其尺寸和其自动化的流程适用于涂层的批量生产。
附图说明
在下面的说明书和附图中详细阐释本发明的实施例。所述附图在示意性视图中示出:
图1燃料喷射嘴的喷嘴体的保持在剖面中的部分视图,具有设置在喷嘴体的突出区域中的喷射孔,
图2金属构件的层构造的剖面示图,该金属构件具有衬底、施加在所述衬底的表面上的粘附层、施加在粘附层上的渐变层和施加在上方的功能层,
图3A具有在真空腔中运行的根据本发明的用于涂覆金属构件的方法的主要方法阶段的流程图,
图3B具有根据本发明的用于涂覆金属构件的方法的实施方式的主要方法阶段的流程图,所述金属构件具有包括三个层的层构造,和
图4用于实施根据本发明的方法的、具有控制和协调装置的设备的示意性框图,该控制和协调装置与HiPIMS组件以及ECR组件和它们相对应的脉冲发生器共同作用。
具体实施方式
图1示出整体标有10的构件,所述构件根据实施例构造为燃料喷射嘴的喷嘴体,具有布置在喷嘴体的突出区域11中和穿过该喷嘴体的壁的喷射孔12,其中,借助于根据本发明的方法将涂层13既施加到喷嘴体的外面上又施加到喷射孔12的内面上。
图2在横截面视图中示出按照根据本发明的方法涂覆的构件10的典型层构造。在此,在由钢形成的衬底10'的表面上借助于大功率脉冲磁控溅射(HiPIMS:high powerimpulse magnetron sputtering)施加有金属粘附层14。在粘附层14上施加有渐变层(Gradientenschicht)15,该渐变层的构造同样借助于HiPIMS实现。最后,在渐变层15上施加有功能层16,所述功能层典型地涉及非晶含氢碳层(a-C:H)或者硅掺杂的a-C:H层并且所述功能层借助于电子回旋共振等离子体(ECR:“electron cyclotron resonance”)由气相沉积或构造。
图3A示出具有根据本发明的方法的实施方式的主要方法阶段110至150的流程图100,所述方法用于涂覆金属构件,其中,所述方法在真空腔中进行,所述真空腔与另外的部件共同形成用于实施根据本发明的方法的设备。
在基本上用于过程初始化的第一方法阶段110中,将要涂覆的构件与它们的衬底支架引入到真空腔中,在那里固定并且连接到为此设置的电接触件上。
在第二方法阶段120中,根据当前要构造的层类型从两个接收在真空腔中的组件中选择一个组件。这两个组件一方面涉及HiPIMS组件并且另一方面涉及借助ECR等离子体源在脉冲操作模式中运行的等离子体浸没植入组件(下面称为PIII组件)。
在第三方法阶段130中,激活当前选择的组件并且所述组件一直保持激活或者运行,直至构造期望或预先确定的厚度的层。然后使所选择的组件停止工作。
如果选择并且激活、即运行HiPIMS组件,那么借助于辉光放电点燃等离子体,将由相对应的脉冲发生器产生的高压脉冲施加到所述构件上,其中,离子从靶材料朝着布线为对应电极的构件转向并且在那里植入;磁场用于提升沉积率。因此,根据所使用的靶材料可以通过固体沉积构造例如基于Ti、Cr、W、Mo或类似元素的不同性质的金属层。
如果选择并且激活、即运行借助ECR等离子体源运行的PIII组件,那么借助于在电荷载体中的微波共振吸收点燃等离子体,所述电荷载体在磁场轨中环绕,其中,一方面将气体作为前体导入到真空腔中并且另一方面将由相对应的脉冲发生器产生的高压脉冲施加到所述构件上,其中,离子从等离子体导向至设有偏置电位的构件并且在那里植入。如果衬底在脉冲期间短暂地处于接地电位,那么在衬底和等离子云之间构造在德拜长度的范围中的暗区,该德拜长度基本上取决于等离子体密度和电子温度并且针对典型的ECR放电处于十分之一毫米的数量级中,由此对于等离子体可能的是,也跟踪衬底的相对小的结构变化;如果在脉冲期间在衬底上施加负电压脉冲,那么使离子从等离子体朝着衬底冲击式地加速,其中,暗区同时膨胀,直至所述暗区占据相应于恰好作用的电压脉冲的尺寸;在随后的脉冲周期中又发出所述电压,即衬底回到接地电位,由此又重新出现初始状态。由于具有高压脉冲(在0.5至约10千伏的低的千伏范围内)的短脉冲(在微秒范围内)可能的是,同样地涂覆构件和所述构件的孔内壁。
在第四方法阶段140中进行询问,是否应构造另外的层。在得到肯定的询问结果时回到方法阶段120,然后重新选择两个组件中的一个组件,并且随后根据阶段30激活,而在得到否定的询问结果时所述方法转到第五方法阶段150。
在第五方法阶段150中,所述方法结束,其中,将完成涂覆的衬底或构件从真空腔中取出。
图3B示出具有根据本发明的方法的实施变型方案的主要方法阶段210至250的流程图200,所述实施变型方案用于涂覆具有根据图2的层构造的金属构件。
在基本上用于过程初始化的第一方法阶段210中,将衬底支架与布置在其上的并且为了涂覆所设置的构件引入到真空腔或过程腔中,由此所述构件作为三维衬底直接连接到电接触部或接触轨上,所述电接触部或接触轨可以通过控制和协调装置与两个高压脉冲发生器的各一个电作用连接,这两个高压脉冲发生器中的一个高压脉冲发生器对应于HiPIMS组件,而另外的高压脉冲发生器对应于借助ECR等离子体源运行的PIII组件。第一方法阶段210结束,其方式是,将真空腔抽真空,直至达到所需要的过程压力。
在随后的第二方法阶段220期间,根据优选的实施例将可以典型地由氮化铬形成的金属粘附层施加在衬底表面上。为此,通过控制和协调装置激活HiPIMS组件和对应的高压脉冲发生器。第二方法阶段220结束,其方式是,通过控制和协调装置使HiPIMS组件和对应的高压脉冲发生器停止工作。
在根据是否在之前构造的粘附层上施加渐变层可选地形成的第三方法阶段230中,通过控制和协调装置重新激活HiPIMS组件和其高压脉冲发生器,以便由固体相构造渐变层,在该渐变层中金属成分的浓度根据预先确定的型廓(Profil)逐渐下降,以便避免突然过渡到随后的功能层。第三方法阶段230结束,其方式是,通过控制和协调装置使HiPIMS组件和其高压脉冲发生器停止工作。
最后,在第四方法阶段240中,出于防磨损原因将功能层施加在位于下方的层上。因为功能层典型地构造为非晶含氢碳层(a-C:H)或硅掺杂的a-C:H层,不同于前面两个方法阶段120、130,需要选择另外的沉积模式,在该另外的沉积模式中进行由气相的沉积。为此通过控制和协调装置选择并且激活借助ECR等离子体源运行的PIII组件和其高压脉冲发生器;同时开启一个或者必要时开启多个用于将碳氢化合物(例如甲烷、乙炔、异丁烷或类似物)供应至真空腔的气体进入阀,以便使这些气体或气体混合物作为前体以掺杂的方式进入到真空腔中并且由此能够实现非晶碳层在位于下方的层上的沉积。除了常见的碳氢化合物之外,作为前体也适用含硅碳氢化合物(如硅烷),所述含硅碳氢化合物可以通过稀有气体和氢气补充。第四方法阶段240结束,其方式是,通过控制和协调装置使借助ECR等离子体源运行的PIII组件和其高压脉冲发生器停止工作并且同时阻止乙炔到真空腔中的气体供应。
在第五方法阶段250中,结束根据本发明的方法,其中,松脱当前涂覆的衬底的电接触并且将衬底支架与衬底一起从真空腔中取出。
适用于实施根据本发明的方法的设备20(图4)基本上包括构造为真空腔的过程腔21、HiPIMS组件22和借助ECR等离子体源在脉冲操作模式中运行的PIII组件23与相对应的脉冲发生器22'、23',所述设备还包括气体进入供应部或气体进入阀25,通过所述气体进入供应部或气体进入阀可以将稀有气体和用于构造DLC功能层的碳氢化合物导入到真空腔中,所述设备还包括衬底支架(未示出),所述衬底支架可运动地和/或可旋转地构造,并且所述设备包括控制和协调装置24,该控制和协调装置通过电导线24'、24”、24”'与组件22、23和气体阀25共同作用,以便实现三维衬底的连续涂覆。为此控制和协调装置24根据当前要构造的层类型选择和激活两个组件22、23中的一个组件,其中,控制和协调装置24具有切换功能,该切换功能参照附图标记24-1在图4中强烈简化地示出。为了说明,在切换功能24-1的在图4中示出的切换位态中选择HiPIMS组件22,而PIII组件23在该切换位态中切换成非激活。出于物理原因,控制和协调装置24以及对应于组件22、23的脉冲发生器22'、23'布置在真空腔21外部。
总结而言,根据本发明的方法100用于涂覆至少一个金属构件、尤其是至少一个喷射嘴的喷嘴体,其中,所述方法在具有HiPIMS组件和借助ECR等离子体源在脉冲操作模式中运行的PIII组件的过程腔中进行,所述方法具有以下方法步骤:a)根据方法阶段110,将所述至少一个构件作为三维衬底引入到真空腔中,b)根据方法阶段120,根据当前要构造的层类型选择所述组件中的一个组件,c)根据方法阶段130,激活所选择的组件,以便构造具有预先确定的层厚度的层,并且d)必要时重复方法阶段120至130,直至在构件上分别构造不同层类型的层。在用于实施所述方法的设备20的控制和协调装置24的存储区中执行根据图3A和3B的根据本发明的方法的运行程序,使得由此得出尽可能自动的流程,因为控制和协调装置24与HiPIMS组件22以及与PIII组件23和它们相对应的脉冲发生器22'、23'互连并且共同作用,控制和协调装置24还切换并且调节与对应的组件22、23相互配合的气体进入阀25,由此一方面稀有气体并且另一方面用于构造DLC功能层的碳氢化合物可以被导入到真空腔中。因此,总体上能够控制衬底借助至少一个金属粘附层和至少一个DLC功能层的连续涂覆。
Claims (11)
1.用于涂覆至少一个金属构件的方法,其中,所述方法在具有HiPIMS组件和通过ECR等离子体源在脉冲操作模式中运行的等离子体浸没植入组件的过程腔中运行,所述方法具有下列方法步骤:
a)将所述至少一个构件作为三维衬底引入(110)到构造为真空腔的所述过程腔中,
b)根据当前要构造的层类型选择(120)所述组件中的一个组件,
c)激活(130)所选择的组件,以便构造具有预先确定的层厚度的层,并且
d)重复方法步骤b)至c),直至在所述构件上分别构造不同层类型的层。
2.根据权利要求1所述的方法,其特征在于,在选择(120)和/或激活(130)所述等离子体浸没植入组件时将至少一种用作为前体的气体以掺杂的方式导入到所述真空腔中。
3.根据权利要求1或2所述的方法,其特征在于,在方法步骤c)期间,所述至少一个构件通过对应于所选择和激活的组件的脉冲发生器的高压脉冲在配属于所述至少一个构件的衬底支架没有电中间连接的情况下受到电加载。
4.根据权利要求1或2所述的方法,其特征在于,在方法步骤c)期间,所述至少一个构件在所述真空腔中至少暂时地运动。
5.根据权利要求1或2所述的方法,其特征在于,在方法步骤c)期间,所述至少一个构件围绕至少一个旋转轴线至少暂时地旋转。
6.根据权利要求1或2所述的方法,其特征在于,所述至少一个金属构件构造为喷射嘴的至少一个喷嘴体。
7.根据权利要求2所述的方法,其特征在于,所述气体是气体混合物。
8.构件,所述构件根据权利要求1至7中任一项所述的方法涂覆。
9.一种用于涂覆至少一个金属构件的设备,所述设备用于实施根据权利要求1至7中任一项所述的方法,其特征在于,构造为真空腔(21)的过程腔具有HiPIMS组件(22)和通过ECR等离子体源在脉冲操作模式中运行的等离子体浸没植入组件(23),并且与这两个组件(22、23)共同作用的控制和协调装置(24)设置成用于根据当前要构造的层类型选择、激活并且控制这两个组件(22、23)中的一个组件。
10.根据权利要求9所述的设备,其特征在于,所述控制和协调装置(24)在所选择的组件(22、23)中将对应于所选择的组件的脉冲发生器(22'、23')在高压输出侧与所述至少一个构件直接电连接。
11.一种用于涂覆至少一个金属构件的批量设施,所述批量设施包括根据权利要求9或10所述的设备。
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