CN105008584B - 装饰性深黑色涂层 - Google Patents
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Abstract
本发明涉及具有耐磨性的深黑色涂层,其中,在一个零件上首先施加具有高硬度的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。通过由此在梯度层内出现的折射率变化,该梯度层作为减轻反射的层。
Description
技术领域
本发明涉及制造用于装饰性应用的具有深黑色外观的耐磨层的方法。
背景技术
人们大量需要看上去是黑色的表面,例如在消费品领域如钟表壳体、手机或机动车上的保险杠。但在这样的应用中,不仅最好是深黑色的外观扮演了重要角色,而且针对外界机械作用的稳定性也起到作用。该表面尤其应该是耐刻划的。
在德国专利申请DE3639469中描述了一种具有装饰性黑色外观的硬质材料层,其同时具有高耐磨性。该硬质材料层包括由元素周期表第IVa、Va族的元素构成的第一层、包含第一层的元素的氮化物的第二层、包含该元素的碳化物的第三层和由硬质碳层构成的顶层,在这里,相同元素的碳化物晶体被嵌埋在该顶层中。
还知道采用DLC层。它具有黑色外观并具有高硬度。但是,常见的DLC层具有中性灰度值(L*=淡),其在高于40的范围内。在此情况下且在本说明范围内,CIE 1976 L*a*b*颜色空间基于D65标准照明和d/8°(=散射照明和在8°下测量)。作为深黑色表面,与本说明相关地是指具有中性灰度值L*=<40的表面。
DLC层的黑色观感是通过其良好的吸收能力实现的。这是该材料具有相对高吸收系数的结果。但该吸收系数伴随着2.1至2.3之间的高折射率。这导致了在光线照射到DLC涂层的表面时因为折射率在从空气(n=1)过渡至所述层时显著突变而有相当一部分的光被反射并因此造成高的L*值。
现在可以在该表面上设置光学抗反射层。但这样的层基于干涉原理。因此,其反射性能一方面取决于波长,另一方面也取决于入射角。还有就是这种层的反射性能与所实现的层厚密切相关。这可能尤其在待涂覆的构件的几何形状并非为平面时带来严重问题。
因此,人们需要一种硬质表面涂层,其造成最好与视角无关地始终留在的深黑色观感。
发明内容
因此,本发明的任务是提供一种硬质的表面涂层,其造成最好与视角无关地始留在的深黑色观感。
根据本发明所制造的层体系显示出比常见的DLC层更低的L*值。这是如此做到的,即在DLC层上实现密度减小(且由此折射率减小)的梯度层。当梯度层足够厚时,由此实现了在该表面处减少弗雷斯内尔反射(Fresnelreflexion)。例如具有nDLC=2.3的常规DLC表面的反射在光垂直入射时约为16%。这导致了约47的L*值。与此相比,具有n=1.7的表面的反射在光垂直入射时只为7%。因为在梯度层中实现了增大的折射率,故在梯度层内且在过渡至DLC层时基本上不再出现弗雷斯内尔反射。为此,L*只为32。
此时显然的是,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层具有在2和3之间的折射率和/或在40和60之间的中性灰度值L*,更好为在45和55之间的中性灰度值L*。
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,其不小于1500HV或15GPa,最好是不小于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,最好是不小于8GPa。
根据本发明的另一个实施方式,该DLC层的厚度不小于0.5μm。
根据本发明的另一个实施方式,该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。
本发明的用于制造该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。如果有些柔软的梯度层获得刻痕,则至少在其下方的DLC层保持完好无损,并且因为它也是黑色的,故刻痕几乎不引人注目。
在具有更高粗糙度的基材上,甚至可以出现梯度层的耐磨性的提高,因为基材尖峰之间的区域得到了保护。
由于反射减轻效果不是由于干涉效应,故明显减轻了反射的层厚关联性和角度关联性。
为了制造该梯度层,可以考虑常用于制造DLC层的设备。不需要附加装备或附加气体。
现在,将结合工艺描述来举例详述本发明。
附图说明
图1与参照物相对照地示出了用于各种DLC样品的氢浓度。
具体实施例
所述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,将基材偏压保持在900V的恒定值。DLC涂覆要求80分钟。为了涂覆该梯度层,基材偏压连续地从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。但最好连续增大低压电弧放电电流以抵制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,这又导致了折射率的减小。
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)上而测量的硬度等于18GPa。测量值L*等于35。这将对应于在表面处的n=1.85的折射率。还有,红绿系数a*和黄蓝系数b*根据Lab颜色空间的定义来测量。对于a*,测量到-0.5±1的值;对于b*,测量到1±1的值。该层体系显示了出色的耐磨性。
该梯度层的折射率不能被任意减小,因为它对层的总硬度有直接影响。但由于梯度层的减小反射作用不是基于干涉效应,故一旦获得要实现的最低折射率之时,可继续涂覆具有该折射率的梯度层。在之前的例子中,人们例如可以在达到50V基材偏压持续20分钟时,在保持该偏压值情况下继续涂覆,而没有继续增大折射率。
说明书所示的例子涉及这样的梯度层,该梯度层就其成分来看基本对应于该DLC层。但也可能的是,如此获得较小的光学密度,即在进一步的涂覆过程中并以提高的浓度施加了DLC层后,加入了另外一种化学元素或另外多种化学元素,而同时碳浓度减小。在极端情况下,在该表面处的碳含量可以为零。在此以硅或者SiOx为例,其中x>=0。如果例如采取措施以便从DLC层起出现SiOx含量的增大,或许还伴随x的变化,例如从在至DLC层的交界面处的x=0变化为在表面处的x=2,则在该表面处可以实现SiO2层,其具有1.5的折射率。对于垂直入射的光,此时只被反射4%。
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。
利用与应用相关的试验方法来检验具有梯度层的DLC样品的耐磨性,所述试验方法依据James Heal(http://www.james-heal.co.uk/)的磨损试验机“Crockmaster”。在此方法中,涂覆后的样品用1厘米见方的砂纸(3M281Q Wetordry,包含9μm三氧化二铝微粒)打磨。该机器使砂纸在涂有深黑色DLC的样品上以1赫兹频率来回运动。9N载荷被加在砂纸上并且它每500次往复周期后被替换。在6000个往复周期后,没有确定颜色值(L*、a*和b*)的显著变化以及没有确定划痕。与之对比,深黑色(L*35)的TiAlCN PVD层在相同试验条件下已经在1000个往复周期后具有显著的磨损。
Claims (8)
1.一种在零件上的硬质材料层,其中,该硬质材料层包括DLC层,所述DLC层具有至少10GPa的硬度和nDLC>2.1的折射率nDLC,
其特征是,
在DLC层上设置厚度至少为300nm的梯度层,
其中,在该梯度层上实现密度减小且由此折射率减小,从而该梯度层具有折射率梯度,
其中,在至DLC层的交界区内,该梯度层的在30nm范围内求平均的折射率不小于数值2.0;并且在至空气的过渡区内,该梯度层的在30nm范围内求平均的折射率不大于数值1.85。
2.根据权利要求1的硬质材料层,其特征是,在至空气的过渡区内,该梯度层的在30nm范围内求平均的折射率是n=1.7。
3.根据前述权利要求之一的硬质材料层,其特征是,该梯度层的化学成分只在氢含量方面不同于该DLC层的化学成分。
4.根据权利要求1的硬质材料层,其特征是,在该梯度层内实现的折射率梯度按照从DLC层起朝向表面的方式造成单调变小的折射率。
5.根据权利要求1的硬质材料层,其特征是,如此选择该梯度层的厚度,即该表面看上去是深黑色的。
6.一种用于制造深黑色的耐磨表面的方法,其包括以下步骤:
-将待涂覆的基材装入涂覆腔;
-对涂覆腔进行抽吸,并输入工作气体,所述工作气体是由乙炔和氩气构成的组合物;
-产生等离子体;
-施加基材偏压于待涂覆的基材上;
其特征是,
为了设置DLC层,首先施加高数值的基材偏压;并且为了随后涂覆梯度层而减小该基材偏压,所述深黑色的耐磨表面为如权利要求1所述的硬质材料层。
7.根据权利要求6的方法,其特征是,为了随后涂覆梯度层而以连续减小和/或以许多小的减小步骤来减小该基材偏压。
8.根据权利要求6的方法,其特征是,借助低压电弧放电产生等离子体。
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