CN1681745A - 制备层和层系统的方法以及涂敷的基材 - Google Patents

制备层和层系统的方法以及涂敷的基材 Download PDF

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CN1681745A
CN1681745A CNA038217848A CN03821784A CN1681745A CN 1681745 A CN1681745 A CN 1681745A CN A038217848 A CNA038217848 A CN A038217848A CN 03821784 A CN03821784 A CN 03821784A CN 1681745 A CN1681745 A CN 1681745A
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C·默勒
L·贝维格
F·科佩
T·屈佩尔
S·盖斯勒
S·鲍尔
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Abstract

为制备具有功能层的基材，该基材具有高的光学性能和/或高的表面平滑度，特别是低的浊度和显著更低的粗糙度，本发明提供对基材涂敷至少一个功能层的溅射方法，其中涂敷功能层的溅射方法被中断至少一次并施加厚度小于20nm的夹层，本发明还涉及由该方法制备的涂敷的基材。

Description

制备层和层系统的方法以及涂敷的基材
本发明涉及具有高质量光学性能和/或高表面平滑度的层系统的制备方法，和涉及具有高质量光学性能和/或高表面平滑度的涂敷的基材。
对基材涂敷特别光学层以制备光学组件，例如镜子或反射器的方法长期以来是已知的。光学层在对电磁光谱的一定区域中的辐射的作用方面具有非常宽范围的功能。
对基材涂敷特别光学层系统，其中该光学层系统由多个单个功能层组成，特别是由具有高和低折射率的交替布置的层组成，这些涂敷方法对于大量的应用多年来同样是已知的。在此层系统通常用作光干涉膜，它的光学性能由具有高和低折射率的层的材料的选择和因此相应折射率的选择，由单个层的布置和由单个层的厚度的选择确定。基本上根据所需的光学性能和可加工性在使用已知的光学设计规则和设计辅助工具的情况下进行选择。
近年来，PVD(物理气相沉积)工艺和CVD(化学气相沉积)工艺成为用于制备层和层系统的主要工艺，特别是用于光学层和层系统。
CVD工艺用于制备耐火金属和其它金属、碳化物、氮化物和氧化物的层。优点是可以均匀地和采用高纯度水平施加许多具有几乎是理论密度和良好粘合强度的材料，该优点由如下缺点抵消：不存在对于每种所需的层材料合适的反应，基材必须能够承受大多数情况下高的反应温度和也必须对于反应物是化学稳定的。一般情况下，反应期间要求的压力是10-100Pa，因此粒子的自由通路长度相对短和涂敷速率对于工业工艺不是最优的。
现在相反地，PVC工艺特别是溅射工艺的突出之处在于如下事实：宽范围的可涂敷的基材材料是可能的，存在涂敷材料的几乎无限制的选择，可以自由地选择基材温度，层粘合优异和容易通过选择工艺参数影响层的微结构。最初开发的溅射工艺的缺点基本上由各种各样的发展消除了，因此现在溅射技术是最通用的和最广泛使用的涂敷工艺。
近年来，磁控溅射(magnetron sputtering)源的使用和进一步开发表明磁控溅射工艺特别适合用于工业涂敷工艺。磁控溅射工艺允许低压力范围(低至0.1Pa以下)中的高涂敷速率同时保持基材的较少加热。
用于溅射的过程是本领域技术人员基本已知的。
借助于阴极雾化，优选通过磁控管(magnetron)阴极雾化，采用例如在DE4106770中描述的溅射设备涂敷基材。在此，由层起始材料制成的所谓的靶受到在两个电极之间形成的等离子体云的作用，其中靶同时形成阴极。雾化的靶材料具有对于反应性气体的亲合力，和通过与后者形成化合物而在基材上沉积为层。
EP0516436B1描述了用于对基材涂敷一个或多个层的磁控溅射装置。
装置的特定形式有益于更有效的溅射工艺。为此目的，装置含有真空腔，其中存在转鼓形式的基材夹具，和在真空腔的内壁存在由层起始材料制成的靶，在此于磁控管上布置靶。
通过在其上存在基材的转鼓的旋转使得基材被均匀涂敷。此形式的溅射也允许基材由多个层涂敷而不必从真空腔中取出，以及简单地影响层的厚度。
然而，已经发现对于特别采用光学层和层系统涂敷基材的已知的溅射工艺仍然总是出现以混浊和层表面的相对较大的粗糙度的形式存在的质量缺陷，当照亮涂敷的基材时，该层表面可一般被识别为具有扩散的光散射的区域。除具有纯装饰效果以外，混浊也降低涂层的反射度和因此降低反射光学系统的质量。在滤光器光学系统的情况下，此混浊导致透射度的降低。在两种情况下，除光散射的效果以外，增加的吸收也可引起产品质量的降低。
因此，本发明是基于如下目的：提供涂敷基材的方法，该方法可用于施加具有高光学质量和/或高表面平滑度的层和层系统，和提供具有高光学质量和/或高表面平滑度的涂敷的基材。
此目的非常令人惊奇地由权利要求1-10所述的方法和权利要求11-23所述的涂敷的基材达到。
因此，对基材涂敷至少一个功能层的方法包括如下步骤：在真空系统中提供基材和在此真空系统中提供层起始材料，和通过层起始材料的溅射来涂敷基材，其中用于对基材涂敷功能层的溅射方法中断至少一次，以施加与功能层相比非常薄的且与功能层不同的夹层，该夹层的厚度小于20nm。
这样的方法称为溅射，即在该方法中，以固体形式作为靶存在的层起始材料曝露于离子的轰击，从而使得能够发射靶的原子、原子束或分子和因此能够雾化层起始材料。
在本文中以下称作功能层的可以是具有光学活性的(即它们在对电磁光谱的一定区域中的辐射的作用方面具有功能)涂层的单层。在此情况下，涂层可以只由一个功能层组成，或者由多个功能层组成，例如由具有高折射率和低折射率的功能层组成的干涉层系统。
在此描述的对基材涂敷至少一个功能层的方法有利地既不影响已知装置的构造也不影响已知的溅射工艺本身，而是规定了用于功能层制备的新工艺过程，由此可以显著改进其质量。这并不要求对本身已知的装置进行任何变化，而只是使用本身已知的措施根据本发明方法重新组织加工过程。该方法不限于特定的溅射装置，而是可以推广到允许层起始材料溅射的任何装置形式。
由于可以达到比采用其它溅射工艺更高的溅射速率和因此存在经济益处，磁控溅射经证明是特别有利的。
在有利的实施方案中，以一定的方式涂敷基材，从而使得通过在反应性气氛中的溅射，交替施加具有低折射率的功能层和具有高折射率的功能层。在此情况下，由于这些材料特别适用于光学干涉系统，具有低折射率的功能层优选由SiO2组成和具有高折射率的功能层优选由ZrO2组成。
本发明人发现，如果由ZrO2形成的具有高折射率的功能层用由SiO2形成的具有低折射率的非常薄的夹层间隔，可以得到具有显著降低的混浊度的功能层。
依赖于功能层的厚度，这些夹层的厚度为0.1nm-20nm，优选0.5nm-10nm，特别优选1nm-3nm，并且是非光学活性的，即在任何情况下它们低于这样的厚度：在该厚度下它们对于所考虑的电磁光谱区域中的光谱曲线引起显著的变化。
使用此方法制备的功能层显得更明亮和更平滑，并增加了透射度和/或反射度。
根据本发明的方法也适用于对基材涂敷金属层，特别是铬构成的功能层。在此情况下，金属特别是铬构成的功能层的间隔通过引入富氧微波等离子体来实施，可以通过微波施加器产生该等离子体。在此情况下，短时间中断溅射纯金属靶或Cr靶的过程并启动微波施加器，它导致将氧引入真空。此氧与已知施加到基材上的金属层反应，从而形成薄的金属氧化物层，因此形成非常薄的夹层。然后继续金属或铬靶的溅射。以此方式制备的层具有显著更平滑的表面，它同样导致更好的光学性能，以及有益于进一步的加工。
本发明人发现此方法导致使用此方法制备的铬层表面的测量粗糙度仅为在抛光不锈钢样规情况下测量的粗糙度的大约一半，该抛光不锈钢样规是迄今为止优选的制备高度抛光导电表面的方法。
可以任意次数地重复上述涂敷过程的每一个以获得多个具有夹层的功能层，在此不是必须要求通过夹层来间隔每个功能层。
有利的是将基材安装在位于真空腔中的转鼓之上，并旋转经过具有层起始材料的靶和经过氧源。由此保证均匀的涂敷。
对本领域技术人员显然的是其它合适的设备同样也可用于涂敷操作。
除根据本发明的方法以外，本发明也包括含有至少一个由金属形成的功能层的涂敷的基材，其中功能层由夹层间隔至少一次，在此夹层由金属氧化物组成且厚度小于10nm。
特别是对于其功能层是铬层的基材，如果通过金属氧化物组成的夹层，特别是通过氧化铬层间隔功能层，那么证明这对于表面平滑度是有益的。
采用铬如此涂敷的基材例如用作平版印刷工艺的基材。
另一种根据本发明的涂敷的基材被打算用作光学元件，例如，用于数字投影的滤色器。
基材的涂层在此情况下由下列部分组成，即至少一个金属氧化物组成的功能层，和至少一个间隔功能层的金属氧化物组成的夹层。在此情况下，夹层的厚度小于夹层具有光学活性时的厚度。
单个功能层优选是具有低折射率的功能层和具有高折射率的功能层，其中功能层用至少一个由金属氧化物组成的夹层间隔。在此情况下，将由SiO2形成的具有低折射率的夹层引入由ZrO2形成的具有高折射率的功能层。
由于以此方式配置的基材涂层具有上述的良好光学性能，因此它们用于许多领域。
采用此方式涂敷的基材不依赖于已知的溅射工艺，和也可以想得到使用其它工艺，例如使用CVD工艺来制备它们。
在此公开的方法仅表示通过其可制备本发明的涂敷的基材的可能有利方法。
以下根据优选的实施方案和参考附图更详细地解释本发明。在此图中相同的参考符号表示相同或相似的部件。在附图中：
图1：图示采用SiO2和/或ZrO2涂敷基材的磁控溅射设备。
图2：图示采用Cr涂敷基材的磁控溅射设备。
图3：图示通过根据本发明一个实施方案的层系统的横截面。
图示不按比例；对于各个应用情况原则上可以自由选择层的厚度和层厚度相互之间的比例。
例示的实施方案
图1显示图解说明的磁控溅射设备，该设备可用于对基材涂敷具有高和低折射率的功能层。
此类型磁控溅射设备的基本结构从EP0516436B1中是已知的，因此在下文中不再详细描述。
在真空腔(5)的内部存在转鼓(7)，将要涂敷的单个基材(1)固定到转鼓上。另外，所示磁控溅射设备在该实施例中的环形内壁(6)之上具有四个溅射电极单元(10a，11a)，以及泵(9)和两个微波产生器(8)。已经发现EP0516436B1中描述的装置非常适合用于本发明的基材涂敷，但方法不限于此具体装置，而是也可以在其它溅射装置上进行。
在制备具有金属氧化物层的蓝色滤色器的优选实施方案中，在真空腔内部的转鼓(7)上放置多个基材(1)。
为了对基材(1)涂敷由具有高折射率的ZrO2和具有低折射率的SiO2组成的交替层系统，在该交替层系统中第一ZrO2层的厚度大约为93.3nm，通过Zr靶(10b)的溅射将Zr原子引入真空腔(5)，这些Zr原子与从微波产生器(8)放入的氧反应性气体反应而形成ZrO2，并以14.1nm ZrO2/分钟的涂敷速率在205s之后形成功能层的第一分层。在此之后，进行Si靶(11b)的Si原子反应性溅射4s的短时间。在首先施加的ZrO2功能层上，产生的SiO2以25.7nm SiO2/分钟的涂敷速率沉积为夹层。
在此情况下，对于施加SiO2组成的夹层，只是4s的短涂敷持续时间导致1.7nm的夹层计算厚度。
然后，再次在反应性气氛中从Zr靶(10b)溅射Zr以制备仍然还不存在的第一功能层的第二个半部分。
在下一步骤中，施加另一个具有低折射率的功能层。此层由氧化硅组成，采用25.7nm SiO2/分钟的涂敷速率，从Si靶(11b)作为Si原子反应性地溅射入真空腔(5)中。此SiO2同样沉积在先前施加的层上。在此步骤中，涂敷操作的持续时间也依赖于要涂敷的层的厚度。
显然的是，如果需要，由SiO2形成的功能层也可以用非常薄的ZrO2夹层分隔。
依赖于应用情况，可能必需施加多个交替层系统以达到交替层系统，如蓝色滤色器的预期的光学效果。采用此方式在这样的交替层系统中分隔多个层是十分显而易见的。
图2显示另一个磁控溅射装置的实施方案，该装置用于根据本发明在用于平版印刷工艺的基材上制备铬层。它在结构上相应于图1中显示的磁控溅射装置，但仅含有两个溅射电极单元(12a)。
在真空腔(5)内部的转鼓(7)上提供基材(1)。为向基材(1)施加铬组成的第一功能层，通过Cr靶(12b)的金属溅射将Cr原子引入真空腔(5)中。
在此，关键的是在真空腔(5)中不存在氧或不引入氧。进行溅射工艺直到达到所需的铬层厚度，在此情况下为30nm。然后，关闭溅射电极单元(12a)和短时间启动微波产生器(8)，由此在真空腔(5)中形成氧等离子体，它氧化新溅射的金属铬表面。形成的氧化物层厚度是如此薄，从而使得它对镜面层的光谱性能，特别是反射性能不具有影响。
在此操作之后，关闭微波产生器(8)和再次激活溅射电极单元(12a)，从而通过Cr靶(12b)的金属溅射施加另一个大约30nm的铬层。重复此过程直到达到270nm的所需总厚度。
图3图示根据上述方法涂敷有功能层(2)的基材。在此情况下，将功能层(3)的第一个半部分施加到基材(1)上，随后由夹层(4)间隔，并在其上施加功能层(3)的第二个半部分。依赖于应用情况和光学设计的预先规定，相互叠加地施加多个如此分隔的功能层(2)，包括不同的功能层，是相当显而易见的。

Claims (23)

1.一种采用至少一个功能层(2)涂敷基材(1)的方法，包括如下步骤：
a)在真空系统(5)中提供基材(1)和层起始材料，和
b)通过层起始材料的溅射对基材(1)涂敷功能层(2)，其特征在于，
b1)中断用于对基材(1)涂敷功能层(2)的层起始材料的溅射至少一次并制备夹层(4)，它不同于功能层且厚度为≤20nm，
b2)在中断之后继续层起始材料的溅射。
2.权利要求1的涂敷基材(1)的方法，其特征在于，通过层起始材料的磁控溅射实现对基材(1)涂敷功能层(2)。
3.权利要求2的涂敷基材(1)的方法，其特征在于，通过如在EP0516436B1中所述的磁控溅射工艺施加功能层。
4.前述权利要求中任一项的涂敷基材(1)的方法，其特征在于施加多个功能层(2)，特别地作为由具有低折射率的功能层(2)和具有高折射率的功能层(2)组成的交替层系统。
5.权利要求4的涂敷基材(1)的方法，其特征在于，具有低折射率的功能层(2)由溅射具有高折射率的夹层(4)间隔和/或具有高折射率的功能层(2)由溅射具有低折射率的夹层(4)间隔，其中夹层保持在它们变成具有光学活性的厚度以下，优选≤10nm。
6.权利要求5的涂敷基材(1)的方法，其特征在于，通过在反应性气氛中溅射硅，具有低折射率的功能层(2)和具有低折射率的夹层(4)由SiO2组成，和通过在反应性气氛中溅射锆，具有高折射率的功能层(2)和具有高折射率的夹层(4)由ZrO2组成。
7.权利要求1-3中任一项的涂敷基材(1)的方法，其特征在于，通过溅射金属施加纯金属层作为功能层(2)。
8.权利要求7的涂敷基材(1)的方法，其特征在于，通过向真空腔中引入富氧微波等离子体而中断功能层(2)的溅射，其中通过先前生长成的由金属组成的功能层(2)的表面氧化而形成由金属氧化物组成的夹层(4)。
9.权利要求8的对基材(1)涂敷功能层(2)的方法，其特征在于，通过溅射铬施加功能层(2)。
10.前述权利要求中任一项的涂敷基材(1)的方法，其特征在于，在位于真空腔内部的转鼓(7)上，基材(1)旋转经过包括层起始材料的靶(10，11，12)和氧源(8)。
11.一种含有至少一个由金属形成的功能层(2)的涂敷的基材(1)，其特征在于，功能层(2)含有至少一个由金属氧化物形成的夹层(4)，该夹层(4)间隔功能层(2)且厚度是≤10nm。
12.权利要求11的涂敷的基材(1)，其特征在于，功能层(2)是铬层。
13.权利要求11-12中任一项的涂敷的基材(1)，其特征在于，由金属氧化物形成的间隔性夹层(4)是氧化铬层。
14.权利要求11-13中任一项的涂敷的基材(1)，其特征在于，它可以由权利要求7-10的方法制备。
15.权利要求11-14中任一项的涂敷的基材，其特征在于，它用作平版印刷工艺的基材。
16.一种含有至少一个由金属氧化物形成的功能层(2)的涂敷的基材(1)，其特征在于，功能层(2)含有至少一个由金属氧化物形成的夹层(4)，该夹层(4)间隔功能层(2)且保持在它具有光学活性的厚度以下。
17.权利要求16的涂敷的基材(1)，其特征在于，它包括由具有高折射率的功能层和具有低折射率的功能层组成的交替层系统。
18.权利要求17的涂敷的基材(1)，其特征在于，具有低折射率的功能层(2)由SiO2组成和具有高折射率的功能层(2)由ZrO2组成。
19.权利要求18的涂敷的基材(1)，其特征在于，在由ZrO2形成的具有高折射率的功能层(2)中由金属氧化物形成的间隔性夹层(4)是由SiO2形成的具有低折射率的夹层(4)，和在由SiO2形成的具有低折射率的功能层(2)中由金属氧化物形成的间隔性夹层(4)是由ZrO2形成的具有高折射率的夹层(4)。
20.权利要求16-19中任一项的涂敷的基材(1)，其特征在于，它可以由权利要求4-6的方法制备。
21.权利要求16-20中任一项的涂敷的基材，其特征在于，它用作光学元件。
22.权利要求21的涂敷的基材，其特征在于，它用作滤色器。
23.权利要求11-22中任一项的涂敷的基材，其特征在于，功能层是光学功能层。
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