CN105683409A - 装饰性hipims-硬材料层 - Google Patents
装饰性hipims-硬材料层 Download PDFInfo
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Abstract
本发明涉及在真空涂覆室中进行的用装饰性硬材料层涂覆基底的方法，其中借助反应性HIPIMS法沉积该装饰性硬材料层，且其中调节功率脉冲中的能量含量以使沉积的硬材料层具有均匀颜色、高光滑度和高硬度。
Description
本发明涉及在真空涂覆室中进行的用装饰性硬材料层涂覆基底的方法，其中借助反应性HIPIMS法（高功率脉冲磁控管溅射）沉积该装饰性硬材料层，并其中调节功率脉冲中的能量含量以使沉积的硬材料层具有均匀颜色、高光滑度和高硬度。
现有技术
专利文件US4415421A描述了制造装饰性金色层的方法，其包括借助电子束蒸发沉积TiN的可承载的（tragf?hig）保护层和借助金的蒸发在该TiN层的表面上沉积金层。
专利文件EP0201508B1描述了由金掺杂的金色TiN层及其制造方法。
但在专利文件DE3134587C2中提出，对于实际应用，金不是非常适合作为制造金色薄膜的材料，因为其一方面非常昂贵，另一方面不具有良好耐磨性并因此容易受损。因此，在DE3134587C2中建议使用具有Cu-Sn-Al-合金的金色层代替金的金色层的涂层。该金色Cr-Sn-Al-层应施加在最初涂层和最终涂层之间。可以根据DE3134587C2通过分别借助喷涂或刷涂施涂聚酯、丙烯酸树脂或聚氨酯之类材料的漆料，此后加热，然后干燥并实现预定厚度，从而制造最初涂层和最终涂层以。对于最终涂层，应使用透明漆料。
在公开文件DE3150039A1中描述了不必使用金作为层材料制造金色涂层的另一可能性。根据DE3150039A1，由TiN和ZrN制造具有良好耐磨性的无金的金色层。
类似地，DE3731127C2建议装饰性涂覆基底的方法，其中借助Ti、Zr或TiZr-合金的靶的阴极电弧蒸发来沉积金色层，由此在含有氮气的反应性气氛中进行该涂覆，且其中该靶相对于阳极具有负极性。DE3731127C2教导了通过使用TiZr-合金靶和氮气，可以制造组成为TixZr1-xN（其中0<x<1）且其颜色外观随x而变的金色层。此外，DE3731127C2教导了通过使用Ti靶和氮气作为反应性气体和此外含O2和/或C的气体作为掺杂气体，可以制造由O2和/或C掺杂且其颜色外观随相对掺杂含量而变的金色TiN层。另外，DE3731127C2教导了通过使用Zr靶和氮气作为反应性气体和此外含O2和/或C的气体作为掺杂气体，可以制造由O2和/或C掺杂且其颜色外观随相对掺杂含量而变的白金色ZrN层。
专利文件EP1614764B1描述了具有金色涂层的装饰性物件，其颜色通过沉积交替的TiN-和ZrN-层的多个重叠对得以实现，且其中在该涂层中的Zr重量与Zr和Ti重量之和的比率为50%至80%。一方面，该多层结构负责提供符合金2N18或1N14或3N18的颜色，另一方面该多层结构使得当最外层磨损时仍能够保持该颜色外观。在EP1614764B1中还提到，在物件上沉积装饰性层的方法应优选是溅射法，其中使用含Ti和Zr的溅射源。
R.Hallmann在其硕士论文“AStudyofTiNCoatingsonMedicalImplantsDepositedbyHiPIMS”（在瑞典TechnisheUniversit?tofLule?in大学进行）中报道，他借助HIPIMS已能够制造具有从金黄色至浅棕色的各种颜色外观的TiN层。Hallmann提到，可以确定特定涂层性能例如孔隙率和密度对颜色外观的显著影响，以及发现在颜色外观与氧含量之间的微弱关联。
在期刊SurfaceandCoatingsTechnology116-119(1999)278-283中，Roquiny报道了氮气流量对通过使用反应性溅射法所沉积的TiN层的颜色的影响。据Roquiny所述，随着氮气流量增加，沉积的TiN层的颜色从金属灰经金色变成棕红色。
但是，当借助反应性溅射法或HIPIMS法涂覆时，产生均匀层颜色仍是一个巨大挑战。
当借助反应性溅射法或HIPIMS法涂覆时，通常使用金属靶作为溅射材料源，在此使用至少一种反应性气体，其至少部分地与来自靶表面的材料反应以致由产生自该反应并通常为陶瓷的材料覆盖该靶表面区域。该覆盖度取决于工艺参数，例如非常显著地取决于反应性气体流量。这种现象通常被称作靶中毒。据说，当靶表面完全被覆盖时，该靶完全中毒。
基本上，靶中毒对于借助反应性溅射法或HIPIMS法制造装饰性层而言是一个严重问题，因为在这样的方法中，靶中毒通常导致在工艺参数方面出现迟滞行为并通常导致工艺不稳定性。
因此，借助反应性溅射法或HIPIMS法工业制造具有均匀层颜色的装饰性层并不经济，当应使用具有大尺寸的涂覆室时尤其不经济，因为在这种情况下，沿涂覆室分布的涂覆的基底中所得的涂层颜色的不均匀性甚至更大。
此外，当使用HIPIMS法时的额外问题在于，由于所用溅射功率的脉冲式变化，在涂覆过程中在涂覆室中发生反应性分压的波动，这也造成所得层颜色的不均匀性。
发明目的
本发明的目的是提供用装饰性硬材料层涂覆基底表面的方法，其一方面为该涂覆的表面赋予耐久的有色外观，另一方面实现容易设定均匀的颜色外观。
发明描述
通过提供根据权利要求1的方法，实现本发明的目的。
本发明人已发现，如果在HIPIMS法中使用具有每功率脉冲和/或每功率脉冲序列至少，优选大于0.2焦耳/cm2的基于所述靶表面计的能量含量的功率脉冲和/或功率脉冲序列，能够令人惊讶地借助反应性HIPIMS法制造具有非常均匀颜色外观、非常高硬度和非常光滑层表面的硬材料层，其由于这些层性能特别地极其适用于装饰性应用。功率脉冲序列被理解为是指功率脉冲群。
图4展示了在靶处可能的功率曲线的示例性图示，以更好理解本发明范围内使用的术语。
术语“具有基于所述靶表面计的能量含量的功率脉冲或功率脉冲序列”在本发明范围内被理解为是指在功率脉冲1的脉冲持续时间t脉冲的过程中或在功率脉冲序列3的序列持续时间t脉冲序列的过程中输入靶表面的总能量含量，其中将在功率脉冲1的脉冲持续时间t脉冲的过程中或在功率脉冲序列3的序列持续时间（脉冲群持续时间）t脉冲序列的过程中等离子体有效投射在其上的靶表面作为靶表面。该靶表面通常被称作“跑道（Racetrack）”并可以在靶处被认为是蚀刻表面（Abtragfl?che）。
可以例如通过设定相对非常高的脉冲功率P和/或相对非常长的脉冲长度或脉冲持续时间t脉冲实现在HIPIMS法中根据本发明在功率脉冲1中必需的能量含量。当然只能将相应的脉冲功率P和脉冲持续时间t脉冲设定为如此大，以使相应的涂覆室装置中的靶材料不会热超载。以类似方式，可以通过设定在功率脉冲序列3内形成序列或脉冲群的脉冲的脉冲功率P和/或通过设定功率脉冲序列3的序列持续时间t脉冲序列来实现根据本发明在功率脉冲序列3中必需的总能量含量。
根据本发明进行的HIPIMS法非常稳定地进行，并且令人惊讶地，工艺稳定性和由此方式制造的硬材料层的对于装饰性应用而言重要的层性能的均匀性都不由于可能的靶中毒现象和/或反应性分压波动而受损害。
具体地，本发明涉及在涂覆室中涂覆基底表面的至少部分区域的方法或制造具有含装饰性硬材料层的表面区域的基底的方法，其中为了制造该硬材料层，使用反应性HIPIMS法，其中使用至少一种反应性气体和使用至少一个可在HIPIMS法的进行过程中与该反应性气体反应的材料靶以由此产生预定的层颜色，其中通过使用具有每功率脉冲和/或每功率脉冲序列至少，优选大于0.2焦耳/cm2的基于所述靶表面计的能量含量的功率脉冲和/或功率脉冲序列进行该HIPIMS法并由此产生硬材料层的均匀颜色外观。
不能排除的是：包括满足这些要求的功率脉冲和/或功率脉冲序列（功率脉冲群）在内，还可以使用不满足所提到的要求，即关于能量含量的要求的功率脉冲和/或功率脉冲序列（功率脉冲群）。在此可以猜测，施加的功率脉冲和/或功率脉冲序列的至少50%应满足所提到的要求。在如今的实现方式中，几乎所有的功率脉冲和/或功率脉冲序列都满足所提到的要求或仍有待提出的更尖锐的要求。
此外，可以用功率脉冲和用功率脉冲序列使用混合操作。
此外指出，靶的热负载包括通过脉冲功率和脉冲持续时间或通过单个脉冲功率和序列持续时间（脉冲群持续时间）在内还通过所选占空比，即通过以下因素来确定：
·功率脉冲的脉冲持续时间(开启时间)与脉冲周期(开启时间+关闭时间)的比率或
·脉冲群-（序列）持续时间与脉冲群周期（脉冲群开启时间+脉冲群关闭时间）的比率。
优选引入每功率脉冲和/或每功率脉冲序列至少，优选大于0.2焦耳/cm2的能量含量，其中通过设定至少，优选大于100W/cm2的功率密度，优选在至少，优选大于0.2A/cm2的电流密度下。
根据本发明的一个优选的实施方案，通过使用具有每功率脉冲和/或每功率脉冲序列至少，优选大于1焦耳/cm2的基于所述靶表面计的能量含量的功率脉冲和/或功率脉冲序列进行该HIPIMS法。
优选通过设定至少，优选大于500W/cm2的功率密度，优选在至少，优选大于1A/cm2的电流密度下，引入每功率脉冲和/或每功率脉冲序列的该能量含量。
根据本发明的一个特别优选的实施方案，通过使用具有每功率脉冲和/或每功率脉冲序列至少，优选大于10焦耳/cm2的基于所述靶表面计的能量含量的功率脉冲和/或功率脉冲序列进行该HIPIMS法。
优选通过设定至少，优选大于1000W/cm2的功率密度，优选在至少，优选大于2A/cm2的电流密度下，引入该能量含量。
优选地，通过调节（控制或调整）反应性气体流量来控制涂覆室中的反应性气体浓度。
下面借助若干实施例和图1至3进一步描述本发明。
图1展示了由根据本发明制造并在提高的氮气气体流量或在提高的乙炔气体流量下沉积的TiN-和TiCN-层测量的CIELab色坐标a*和b*。通过设定各种氮气气体流量，可以制造具有各种金标准的TiN层。以类似方式，通过设定各种乙炔气体流量，可以制造具有各种颜色的TiCN层。
图2展示了由根据本发明沉积并在相同涂覆批次中由Ti靶和通过使用含N2和C2H2的反应性气体流量在不同基底上施加的TiCN层测量的CIELab色坐标a*和b*和亮度因数L*。在开始本发明的涂覆方法前，沿涂覆室的高度分布所述基底，以检查沿涂覆室的高度的颜色外观的均匀性。可以证实涂覆室内非常好的层颜色均匀性。涂覆高度或对于涂覆基底所特定的涂覆室高度在该实施例中为400毫米，但是为了进行本发明的方法，涂覆高度不受限于该高度，即涂覆高度可以更小或更大。
图3展示了由根据本发明沉积并在相同涂覆批次中由TiN靶和通过使用含N2的反应性气体流量在不同基底上施加的金色TiN层测量的CIELab色坐标a*和b*和亮度因数L*。在开始本发明的涂覆方法之前，沿涂覆室的高度分布所述基底，以检查沿涂覆室的高度的金色颜色外观的均匀性。可以证实涂覆室内非常好的层颜色均匀性。涂覆高度和对于涂覆基底所特定的涂覆室的高度在该实施例中也为400毫米，但是为了进行本发明的方法，涂覆高度不受限于该高度，即涂覆高度也可以更小或更大。
如在图2和3中可以看出，对根据本发明沉积的TiCN-和TiN-层可以证实沿整个涂覆高度的出色的颜色外观均匀性。
通过使用本发明的方法也可以出色地制造多个交替沉积的薄TiN-和ZrN-层的多层层结构的金色层。例如，这通过在相同HIPIMS涂覆法中使用氮气作为反应性气体并将至少一个Ti的HIPIMS靶和Zr的HIPIMS靶定位于该涂覆室中和促使在待涂覆的基底上交替沉积TiN-和ZrN-层。
根据本发明，通过设定不同的氮气流量，可以非常容易地在根据本发明沉积的硬材料层的情况下制造金标准的各种颜色，这尤其是在使用含Ti靶或优选由钛构成的靶时。
根据本发明，可以准确调节氮气流量以使颜色外观优选符合根据金2N18或1N14或3N18的颜色。
本发明人已确定，通过使用包含钛或钛和铝或锆的靶，尤其可以制造用于装饰性应用的具有美丽颜色的硬材料层。
根据本发明的方法的一个优选实施方案，使用至少一个由钛或由钛和铝或由锆构成的靶。
为了制造可以为根据本发明制造的层提供各种层性能和颜色外观的氮化物、氧化物、碳化物、氮氧化物或碳氮化物，可以将氮气或氧气或含碳气体例如C2H2或CH4或它们的混合物例如N2和C2H2送入用于进行该HIPIMS法的涂覆室。
优选将本发明的涂层施加到其中硬材料层应具有装饰性功能的基底上。
在此所述的本发明的方法特别并极其适用于涂覆作为基底的可由不同材料构成的不同装饰性物件。在使用本发明的方法制造装饰性硬材料层时的一个非常显著的优点在于，还能够涂覆例如不能暴露在高于200℃的温度下的对温度敏感的基底。这是可行的，因为可以选择功率脉冲持续时间t脉冲或功率脉冲序列内的单个脉冲的持续时间或功率脉冲序列持续时间t脉冲以及相应的脉冲间歇（占空比）和决定性的靶表面，以使在该涂覆方法的过程中可以保持非常低的涂覆温度，即非常低的基底温度而不出现工艺不稳定性，从而可以进行本发明的HIPIMS法。
根据本发明，通过设定相应的氮气流量，可以制造具有金标准的各种颜色的硬材料层，但也可以制造其它硬材料层，其颜色外观可以在大的涂覆范围内通过设定相应使用的反应性气体流量或不同反应性气体的浓度来调节。
在本发明的范围内，例如根据本发明制造具有预定颜色和极均匀颜色外观、非常高硬度和超光滑表面的装饰性硬材料层。所用反应性气体流量以及所制造的硬材料层的测量的机械性能记录在表1中。所有方法在150℃至500℃的基底温度下进行。
表1：为了达到用于装饰性应用的各种预定均匀颜色所使用的反应性气体流量和根据本发明沉积的TiN-、TiCN-和TiC-硬材料层的机械性能
| 实施例 | Ar [sccm] | N2 [sccm] | C2H2 [sccm] | 硬度HIT [GPa] | E-模量 [GPa] |
| 1 | 210 | 50 | 0 | 33 | 420 |
| 2 | 210 | 50 | 6 | 32 | 440 |
| 3 | 210 | 50 | 14 | 37 | 400 |
| 4 | 210 | 30 | 20 | 36.3 | 450 |
| 5 | 210 | 40 | 20 | 44 | 462 |
| 6 | 210 | 20 | 24 | 38.3 | 426 |
| 7 | 150 | 30 | 30 | 42.4 | 465 |
这些硬材料层的极高机械稳定性或硬度和E-模量的极好组合使得这些层能够为用其涂覆的物件赋予耐久的有色外观。
这些层具有与基底的极好粘附性并具有极高耐磨性。因此，这些装饰性硬材料层可以使用数年之久。
即使当基底具有非常大的待涂覆表面时，根据本发明的方法也能够达到非常均匀的颜色外观。
当必须沿大涂覆室的高度分布多个基底并应在所有基底上实现均匀颜色外观，根据本发明的方法尤其有利。
Claims (15)
1.在涂覆室中涂覆基底表面的至少部分区域或制造表面区域具有装饰性硬材料层的基底的方法，其中采用反应性HIPIMS法制造所述硬材料层，其中使用至少一种反应性气体并使用至少一个可在所述HIPIMS法的进行过程中与所述反应性气体反应的材料靶以由此产生预定的层颜色，其特征在于：通过使用具有每功率脉冲(1)和/或每功率脉冲序列(3)至少0.2焦耳/cm2的基于所述靶表面计的能量含量的功率脉冲和/或功率脉冲序列进行所述HIPIMS法，并由此产生所述层的均匀颜色外观。
2.权利要求1的方法，其特征在于：在所述功率脉冲和/或功率脉冲序列中基于所述靶表面计的能量含量为每功率脉冲(1)和/或每功率脉冲序列(3)至少1焦耳/cm2。
3.根据前述权利要求之一的方法，其特征在于：在所述功率脉冲和/或功率脉冲序列中基于所述靶表面计的能量含量为每功率脉冲(1)和/或每功率脉冲序列(3)至少10焦耳/cm2。
4.根据前述权利要求之一的方法，其特征在于：通过调节每功率脉冲序列(3)的功率密度，引入在所述功率脉冲和/或功率脉冲序列中基于所述靶表面计的能量含量。
5.根据前述权利要求1至3之一的方法，其特征在于：通过调节所述功率脉冲持续时间(t脉冲)和/或功率脉冲序列持续时间(t脉冲序列)，引入在所述功率脉冲和/或功率脉冲序列中基于所述靶表面计的能量含量。
6.根据权利要求4或5之一的方法，其特征在于：设定至少100W/cm2的功率密度。
7.权利要求6的方法，其特征在于：设定至少500W/cm2的功率密度。
8.权利要求7的方法，其特征在于：设定至少1000W/cm2的功率密度。
9.根据前述权利要求之一的方法，其特征在于：所述基底温度保持如此之低，以使可以涂覆不能暴露在高于200℃或甚至更低的温度下的对温度敏感的基底。
10.根据前述权利要求之一的方法，其特征在于：使用氮气、氧气或含碳气体或它们的混合物作为反应性气体。
11.根据前述权利要求之一的方法，其特征在于：所述靶包含钛或钛和铝或锆。
12.根据前述权利要求之一的方法，其特征在于：所述靶由钛或由钛和铝或由锆构成。
13.权利要求12的方法，其特征在于：所述靶由钛构成并使用氮气作为反应性气体，其中通过调节氮气气体流量控制所述涂覆室中的氮气浓度，并调节所述氮气气体流量以使所述颜色外观符合根据金2N18或1N14或3N18的颜色。
14.使用根据前述权利要求之一的方法制造的硬材料层，其特征在于：所述硬材料层具有至少30GPa的硬度。
15.具有根据权利要求14的硬材料层的装饰性物件。
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- 2014-06-26 WO PCT/EP2014/063611 patent/WO2014207154A1/de active Application Filing
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| CN111448342A (zh) * | 2017-09-15 | 2020-07-24 | 欧瑞康表面处理解决方案股份公司普费菲孔 | 制造具有彩色表面的涂层的方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| WO2014207154A1 (de) | 2014-12-31 |
| MX2015017868A (es) | 2016-08-18 |
| SG11201510649VA (en) | 2016-01-28 |
| US20160369386A1 (en) | 2016-12-22 |
| MY181967A (en) | 2021-01-15 |
| CN105683409B (zh) | 2018-09-07 |
| IL243283B (en) | 2018-11-29 |
| CA2916640A1 (en) | 2014-12-31 |
| PT3013996T (pt) | 2017-07-20 |
| BR112015032334B1 (pt) | 2021-06-15 |
| BR112015032334A2 (pt) | 2017-09-26 |
| PH12015502837A1 (en) | 2016-03-28 |
| BR112015032334A8 (pt) | 2018-01-02 |
| PL3013996T3 (pl) | 2017-10-31 |
| EP3013996A1 (de) | 2016-05-04 |
| KR20160024915A (ko) | 2016-03-07 |
| ES2636867T3 (es) | 2017-10-09 |
| EP3013996B1 (de) | 2017-05-10 |
| US11060181B2 (en) | 2021-07-13 |
| RU2016102152A (ru) | 2017-07-31 |
| JP6426726B2 (ja) | 2018-11-21 |
| JP2016528382A (ja) | 2016-09-15 |
| KR102274981B1 (ko) | 2021-07-09 |
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