CN1323045C - 层系统 - Google Patents

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CN1323045C
CN1323045C CNB038216876A CN03821687A CN1323045C CN 1323045 C CN1323045 C CN 1323045C CN B038216876 A CNB038216876 A CN B038216876A CN 03821687 A CN03821687 A CN 03821687A CN 1323045 C CN1323045 C CN 1323045C
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functional
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titanium oxide
aluminium
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CN1681743A (zh
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克里斯多夫·穆勒
拉尔斯·贝维格
弗兰克·科普
托马斯·库伯尔
斯特凡·盖斯勒
斯特凡·鲍尔
于尔根·齐克
克里斯蒂安·亨
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Schott AG
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Abstract

本发明涉及具有包含氧化钛铝的至少一个层的层系统。包含氧化钛铝的层可以是被或不被在光学上不起作用的中间层所间断的功能层，或者被包含氧化钛铝的中间层所间断的由金属氧化物形成的功能层。层系统在高于600℃的工作温度下在结构和热上稳定。层系统可以仅包含一个功能层或可以是多层系统，优选地由具有高和低折射率的功能层构成的交替层系统。

Description

层系统
技术领域
本发明涉及具有至少一个金属氧化物层的层系统，该金属氧化物包含氧化钛铝。层系统具有高的结构和热稳定性，特别是在超过600℃的工作温度下，并且尤其适合于光学涂层，但并不局限于该特定应用。
背景技术
光学层系统，特别是由相互紧贴的具有高和低折射率的交替薄膜组成的交替层系统，已因广泛应用而知名多年。它们充当光干涉膜，其光学性质由具有高和/或低折射率的层的材料的选择因此相应折射率的选择、各个层的排列，以及各个层厚度的选择来决定。选择基本上是根据期望的光学性质和工艺性能的标准，基于已知的光学设计规则和设计工具。
用于制作例如反射器、镜面、滤波器、灯、IRC喷灯/灯等的该类型涂层的合适起始材料的例子其中包括TiO2和SiO2。
这些材料的薄膜通常通过CVD工艺(CVD＝化学汽相沉积)、PVD工艺(PVD＝物理汽相沉积)或溶胶凝胶工艺来涂敷，并以它们是硬的和化学上稳定的以及具有高的折射率差的事实而著名。
关于对于高温的稳定性，氧化硅应该几乎没有问题。但是，如果氧化钛用作具有高折射率的层材料，则问题在高的工作温度(＞600℃)下出现，该高温可能在例如玻璃陶瓷反射器或IRC灯中达到。氧化钛在这些高温下改变。如由H.Sankur和W.Guning在J.Appl.Phys.66(1989)中广泛描述的，这特别地可归因于在非晶态下涂敷的TiO2的相变。在超过350℃的温度下，Ti02结晶以形成锐钛矿相，然后在大约600℃的温度下形成金红石相。这在涂层中产生混浊，并且已通过特殊光学设计而优化的其光学性质退化。
DE 3227069 A1公开一种光学涂层，其适合于高温并包含由作为具有低折射率的层材料的SiO2和作为具有高折射率的层材料的Ta2O2构成的交替层系统。该涂层能够承受高温并且目的在于提高被涂敷对象特别是卤素灯的工作效率。
与使用TiO2作为具有高折射率的层相比，工作效率的提高和更高的热稳定性确实可以获得，但是在高温范围内使用Ta2O5同样在层中引起相当大的混浊，因此这些涂层不适合于许多应用领域。
发明内容
本发明的一个目的在于提供一种涂层，其在高的工作温度下基本在结构上稳定并保持(实际上)无混浊。
根据本发明的层系统包括由包含氧化钛铝的金属氧化物形成的至少一个层。例如制作层系统的特殊光学设计所需的层系统的各个层在下面称作功能层。
由氧化钛铝形成的功能层具有比已知的由金属氧化物形成的功能层显著更高的热和结构稳定性。
因为包含氧化钛铝的功能层固有地保证高的热稳定性，由另外金属氧化物形成的中间层的额外间断有助于使对象达到它们能够更稳定化的程度，但主要是用来进一步提高包含氧化钛铝的功能层的机械和光学性质。为了避免来自中间层的光学上的不良影响，中间层的厚度或折射率将被选择，以使该层在光学上不起作用。除了它们高的热稳定性以外，作为例子，该类型的层还具有高亮度，导致所期望的光学特征值，例如反射率或透射率的提高，以及高的抗划痕性。
根据本发明的另一种层系统同样地包含由金属氧化物形成的至少一个功能层，其中包含氧化钛铝的至少一个中间层间断由不同于中间层的金属氧化物形成的至少一个功能层。在这种情况下，中间层的厚度或折射率将被选择，以使该层在光学上不起作用。
通过用包含氧化钛铝的中间层来间断由金属氧化物形成的功能层的形态，同样地可能获得由金属氧化物形成的功能层的所期望的热和结构稳定性。此外，用这些中间层的间断使得由金属氧化物形成的功能层的机械和光学性质可以显著改善。这开辟了根据本发明的层系统的广阔应用领域。
以形成在高的热负载下不经历它们结构的任何改变的子层这样一种方式来间断功能层是有利的。例如，其各个子层保持在50nm厚度以下的由金属氧化物形成的非晶功能层在高温作用下不受到任何结晶化。
本发明的一个特别效果是通过设置铝和钛的数量比来设置包含氧化钛铝的层的折射率的可能性。折射率n可以在1.55≤n≤2.50的范围内变化。增加铝含量将减小层的折射率n。更少量的铝(例如Al∶Ti大约为1∶3.84；n＝2.34)显著地提高功能层的结构稳定性和热稳定性。这使得这些层在使用中非常灵活。
设置包含氧化钛铝的层的折射率的能力可以特别有利地用来使功能层的折射率与中间层的折射率相匹配，反之亦然。因此，由具有在1.55≤n≤2.50范围内的折射率n的金属氧化物(例如n大约为2.1的氧化锆或已通过稳定剂材料例如氧化钇等的添加而稳定化的稳定化氧化锆)形成的功能层可以用由氧化钛铝形成的中间层来间断，而不会在光学上受其影响。在这种情况下，中间层不再必须具有必须保持在它们会变得在光学上起作用的厚度以下的具有不同折射率的中间层的低厚度。类似的陈述同样适用于氧化钛铝功能层被金属氧化物所形成的中间层的间断。
根据本发明的层系统可以包括单个功能层或具有多个功能层的层系统，优选地由具有高和低折射率的功能层形成的交替层系统。
在这种情况下，交替层系统由包含氧化钛铝作为具有高折射率功能层的功能层构成并且氧化钛铝功能层由中间层间断，或功能层由氧化钛铝中间层部分间断并且由高折射率的金属氧化物形成同样是可能的。
在交替层系统由具有高和低折射率的功能层形成的根据本发明的层系统的一种优选实施方案中，具有高折射率的功能层包含氧化钛铝。其优选地包含TixAl1-xOy，0＜x＜1，优选地0.3＜x＜1，特别有利地0.5＜x＜1。铝的水平越低，功能层的折射率变得越高。然后低折射率的功能层包含氧化硅，优选地二氧化硅。二氧化硅同样地能够承受高温并具有与氧化钛铝相比低的折射率。
关于光学设计，某种层结构按照功能层的顺序和厚度来预先确定。相应的光学层厚度n*d数量级为 (n＝层的折射率；
Figure C0382168700082
)或更低。对于根据本发明的层系统在近红外和可见区中的应用，功能层的层厚度dF的值则优选地为5nm≤dF≤200nm。用于光学应用的该类型的层系统特别地地适合于在高温范围内即在超过600℃的工作温度下使用。
此外，如果具有高折射率的功能层用具有低折射率的中间层间断，反之亦然，隔开功能层的中间层保持低于它们可能在整个层系统中变得在光学上起作用的厚度是重要的，尤其对于光学层系统。于是中间层的合适厚度dz在0.3nm≤dz≤10nm范围内，优选地在0.5nm≤dz≤4.0nm范围内，特别适当地在1.0nm≤dz≤2.5nm范围内。中间层的使用和层数优选地应当以由功能层形成的子层的厚度dT大约为20nm≤dT≤250nm这样一种方式来选择。因此，待间断的功能层的合适层厚度为dT＝40nm。
关于这点，在由具有高折射率和低折射率的功能层形成的交替层系统中，对于工艺工程顺序，是否具有高折射率的功能层由具有低折射率的层材料所形成的中间层隔开是特别重要的。此外，具有低折射率的功能层由具有高折射率的层材料所形成的中间层间断是可能的。在这种情况下，不绝对必须间断每个功能层。
但是，中间层具有不同于功能层的折射率不是必需的，而是它必须适合于影响功能层中的结构形成，使得高温不会导致涂层的光学性质的任何退化。因此，由例如氧化钛形成的具有高折射率的功能层由氧化钛铝所形成的具有高折射率的中间层隔开也是可能的。
化学汽相沉积工艺，优选地等离子体增强型的，特别地PICVD工艺(PICVD＝等离子体脉冲化学汽相沉积)有利地适合于根据本发明的层系统的制作。
这些工艺允许层的均匀和精确制备，使它们特别地适合于工业涂敷工艺。此外，该工艺可以用来以特别简单的方法来控制铝含量与钛含量的比值。
溶胶凝胶工艺同样有利地适合于涂层的工业制造。
但是，原则上，根据本发明的层系统使用PVD工艺(PVD＝物理汽相沉积)，例如蒸发涂敷、溅射或其他工艺来制造也是可能的。
主要取决于被涂敷目标的应用领域，非常广泛的衬底材料可以使用。对于在高温范围内使用，应当适当地考虑相关的热负载。合适的衬底材料是金属、玻璃和玻璃陶瓷以及塑料。
根据本发明，层系统用于反射器的涂层，特别地用于玻璃陶瓷反射器的涂层。由于涂层的结构和热稳定性，这些涂层使可以获得反射器优越的光学和机械性质，即使在长时间和极端的热负载下。
此外，根据本发明，层系统用于照明体，特别是IRC灯/喷灯的涂层。同样地在这种情况下，由于涂层的结构和热稳定性，这些涂层能够带来在长时间和极端热负载下照明体的优越的光学和机械性质。
附图说明
本发明将在下面基于示范实施方案和附图来更详细地说明，其中：
图1显示用于反射器涂层的根据本发明的层系统。
图2显示在450℃、650℃和750℃的温度下反射器的反射性质。
图3显示在650℃和850℃下处理之后具有不同折射率的氧化钛铝层的衍射图。
图4显示在图3中说明的氧化钛铝层的衍射图的Al∶Ti数量比的一览表。
具体实施方式
图1显示用于反射器的根据本发明的光学层系统。反射器在可见光的波长范围内具有高反射，因此特别地适合于照明用途。由于其在近红外的高透射，以及因而导致的低的热反射，它特别适合于温度密集照明，并且可以例如在数字投影仪中使用。
层系统是交替层系统，并且包含43个功能层。具有低折射率的功能层由SiO2形成，具有高折射率的功能层由TixAl1-xOy形成。
铝和钛的数量比是Al∶Ti＝1∶2.09。在该数量比下，TixAl1-xOy层具有折射率n＝2.26。精确排列和各个层厚度在图1中提供表格中显示。
各个功能层通过PICVD工艺来制造。通过该工艺，本领域技术人员能够以普通方法控制铝含量，使得以对准目标的方式设置氧化钛铝层的折射率是可能的。
以该方法制造的反射器然后暴露于450℃、650℃和750℃的热负载下。在这些热负载之后，反射器不显露任何混浊。
图2显示在上述不同热负载下反射器的反射特征。当测试根据本发明的反射器涂层的反射性质时，证明高的工作温度对反射性质几乎没有任何显著影响，特别地反射器的反射性质在
Figure C0382168700101
的期望波长范围内保持稳定同样地是可能的。同时，反射器在近红外的高透射被保留。
作为例子描述的并具有根据本发明的在结构和热上稳定的涂层的反射器可以在数字投影仪中使用，但也适合于在高电压和低电压技术中的照明用途，例如在卤素照明技术中使用。
此外，根据本发明的各个层的性质被研究。
为了该目的，由石英玻璃制成的衬底通过PICVD工艺在所有情况下被涂敷上一层具有500nm层厚度的TixAl1-xOy单层(0＜x＜1)。铝和钛的不同数量比例在涂敷过程中设置，以便在1.55≤n≤2.50的最小和最大可能值之间改变折射率。在层中设置的比值通过EDX来测量。相应的数量比可以从测量的按at％的比例中确定。钛和铝的按at％的数量比例的各个值，相关的Ti∶Al的数量比以及相应的折射率在图4中所提供的一览表中给出。
铝含量的增加将减小层的折射率n。
然后，被涂敷的衬底暴露于650℃或850℃的热负载下一个小时。在650℃和850℃下处理之后的图3中所说明的各个样品的X射线检查显示：在所有情况下只有具有最低铝含量的n＝2.34的层显露锐钛矿的初始形成。但是，更少量的铝足够防止在高温负载下晶体的形成。与纯的二氧化钛相比，在低温下非晶层的结晶化以形成锐钛矿和在高于600℃的温度下的再结晶化以形成金红石相被抑制。所测量的层不具有任何混浊现象。
因此，已被涂敷上根据本发明的单个功能层的衬底也可以用于非常广泛的应用，优选地高温范围内，因为它们保持在结构上稳定，而没有任何混浊，即使在高于600℃的极端热负载下。
在IRC灯/喷灯上根据本发明的层系统的使用代表另一种可能的应用例子。该情况下的层系统包含由具有高折射率和低折射率的功能层形成的交替层系统。这些干涉层系统典型地包含多于30个功能层。
该类型灯或喷灯的交替层系统的设计是众所周知的。它们使灯所产生的在可见波长范围内的光被透射，而同时产生的IR辐射被反射入发光体内(IRC系＝红外反射涂层)。
被反射的辐射显著地有助于达到发光体的工作温度。灯泡或喷灯的温度可以低于某个环境量至高于1000℃。
到目前为止，已知的交替层系统仅能够承受达到大约600℃的热负载，这特别地可归因于具有高折射率的层的不足的热稳定性。
由氧化铝钛形成的具有高折射率的合适功能层和/或金属氧化物功能层的使用并且中间层在涂层中隔开它们，使得增加IRC灯/喷灯的热稳定性至高于600℃成为可能。

Claims (25)

1.一种层系统，具有至少一个由金属氧化物形成的功能层，该层系统在高于600℃的工作温度下具有高热稳定性，其中由金属氧化物形成的至少一个功能层包含氧化钛铝。
2.根据权利要求1的层系统，其中包含氧化钛铝的至少一个功能层具有至少一个中间层，其间断功能层并由不同于功能层的金属氧化物形成，该中间层在光学上不起作用。
3.根据权利要求2的层系统，其中中间层保持低于其在光学上起作用的厚度。
4.根据权利要求3的层系统，其中中间层的层厚度dz为0.3-10nm。
5.根据权利要求3的层系统，其中中间层包含氧化硅。
6.根据权利要求2的层系统，其中中间层具有与包含氧化钛铝的功能层相同的折射率，使得中间层在光学上不起作用。
7.一种层系统，具有至少一个由金属氧化物形成的功能层，该层系统在高于600℃的工作温度下具有高热稳定性，其中包含氧化钛铝的至少一个中间层间断由不同于中间层的金属氧化物形成的至少一个功能层，该中间层在光学上不起作用。
8.根据权利要求7的层系统，其中包含氧化钛铝的中间层保持低于其在光学上起作用的厚度。
9.根据权利要求8的层系统，其中中间层的层厚度dz为0.3-10nm。
10.根据权利要求8的层系统，其中功能层包含氧化硅。
11.根据权利要求7的层系统，其中功能层具有与包含氧化钛铝的中间层相同的折射率，使得中间层在光学上不起作用。
12.根据权利要求11的层系统，其中功能层包含氧化锆。
13.根据权利要求12的层系统，其中包含氧化钛铝的层包含TixAl1-xOy，其中0＜x＜1。
14.根据权利要求13的层系统，其中包含氧化钛铝的层的折射率n通过钛和铝的数量比而设置于1.55≤n≤2.50。
15.根据权利要求1的层系统，其中该层系统包含多个功能层。
16.根据权利要求15的层系统，其中高折射率的功能层包含氧化钛铝。
17.根据权利要求16的层系统，其中低折射率的功能层包含氧化硅。
18.根据权利要求17的层系统，其中包含氧化钛铝的高折射率的功能层由包含氧化硅的低折射率的中间层间断，和/或包含氧化硅的低折射率的功能层由包含氧化钛铝的高折射率的中间层间断。
19.根据权利要求1的层系统，其中各层通过化学汽相沉积工艺来制造。
20.根据权利要求1的层系统，其中各层通过物理汽相沉积工艺来制造。
21.根据权利要求1的层系统，其中各层通过溶胶凝胶工艺来制造。
22.一种具有包含根据权利要求1的层系统的涂层的照明体。
23.根据权利要求22的照明体，它是红外反射涂层灯或喷灯。
24.一种具有包含根据权利要求1的层系统的涂层的反射器。
25.根据权利要求24的反射器，它是玻璃陶瓷反射器。
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