CN101282916A - 具有中间防散射层的低发射率（低-e）薄膜多层涂层 - Google Patents

具有中间防散射层的低发射率（低-e）薄膜多层涂层 Download PDF

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CN101282916A
CN101282916A CNA2006800305802A CN200680030580A CN101282916A CN 101282916 A CN101282916 A CN 101282916A CN A2006800305802 A CNA2006800305802 A CN A2006800305802A CN 200680030580 A CN200680030580 A CN 200680030580A CN 101282916 A CN101282916 A CN 101282916A
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L·伊洛
U·施米特
R·科姆特斯
H·斯克特
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Abstract

在一种用于透明基材，特别是用于窗玻璃，包括银层作为功能层的高耐热性低发射率(低－E)多层系统中，在基材表面与银层之间，具有高折射层，特别是由TiO2、Nb2O5或TiNbOx制成的，以及在紧靠银层的下面，基本上由ZnO构成的层，在高折射层与ZnO层之间配置了厚度至少是0.5nm、由NiCrOx或InSnOx(ITO)制成、起防散射层作用的混合氧化物层。

Description

具有中间防散射层的低发射率（低-E）薄膜多层涂层
本发明涉及用于透明基材，特别是用于玻璃板的高耐热性低发射率多层系统，具有权利要求1前序部分的特征。
它包含：下抗反射涂层，该涂层具有特别由TiO2、Nb2O5或TiNbOx层制成的高折射层，和基本上由ZnO组成的润湿层，该润湿层连接着以银为基础的功能层，在该银层上面的阻隔层；上抗反射涂层，其由一个层或几个部分层组成；以及覆盖涂层，其由一个层或几个部分层组成；在下抗反射底涂层中，在高折射层与ZnO层之间设置了另外金属氧化物层，其作为防散射层。
一种适合对玻璃板实施的热弯曲和/或增强操作的多层系统，其中以ZnO-为基础的润湿层与二氧化钛层直接相邻被公开在，例如，文献DE197 26 966和文献DE 198 50 023中。然而，据发现，在增强操作后，被此类多层系统散射的光的比例较高。至于可能的原因，据文献EP 1 538131认为，在增强操作期间，在二氧化钛与氧化锌之间的界面发生了导致二氧化钛层破坏的扩散过程。也可以假设，在高温，界面上的扩散过程导致Zn2TiO4的生成，而在结晶状态下，这可能是高比例散射光的成因。
为抑制此种扩散过程，文献EP 1 538 131建议在高折射层与ZnO层之间设置SnO2防散射层。于是，高折射层将在增强操作期间得到保护，因此该层的高折射指数便可得到充分利用，即便在增强操作后。
尽管当设置SnO2防散射层时观察到散射光比例相当大的下降，然而，这一比例依然相当高。另外，发射率更达不到要求的低数值。
本发明基于具有上面提到的基本结构的高耐热性多层系统。本发明的基本问题是进一步改善此种多层系统的性能，特别是进一步降低增强操作后散射光的比例，进一步增加可见光范围的透射，进一步降低表面电阻并因此降低发射值，并在热辐射范围内的反射达到尽可能高的数值。
按照本发明，该问题通过权利要求1中指出的技术特征进行解决。
根据本发明的用于透明基材，特别是用于玻璃板的高耐热性低发射率多层系统，其具有：下抗反射涂层，该涂层具有高折射层；基本上由ZnO组成的润湿层，该润湿层连接着以银为基础的功能层；在该功能层上面的阻隔层；上抗反射涂层，其由一个层或几个部分层组成；以及覆盖涂层，其由一个层或几个部分层组成；在下抗反射底涂层中，在高折射层与润湿层之间设置了另外的金属氧化物层，其作为防散射层。位于高折射层与润湿层之间的防散射层是混合氧化物层，其厚度至少是0.5nm，由NiCrOx或InSnOx(ITO)构成。
术语“高折射层”就本发明的内容而言，应理解为光学指数大于或等于2.2的层。该层优选是非-氮化物层，具体地说是氧化物层。
多层系统的优选组成以及单个层的优选厚度范围将在所附权利要求和下面的说明实施例中给出。
具体地说，高折射层优选由TiO2、Nb2O5或TiNbOx构成。
另外，将高折射层直接配置在玻璃的表面上，或者将介电层，其折光指数n比与它相邻的高折射层的折射指数更小(即小于2.2但又优选大于1.8)置于玻璃表面与高折射层之间，特别是当高折射层由TiO2、Nb2O5或TiNbOx构成时。在这种情况下，置于玻璃表面与高折射层之间的介电层优选地是由SnO2、ZnO、SiO2或Si3N4组成。
优选的是，阻隔层是金属层或由50～80wt％Ti和20～50wt％Al组成的略微氢化的钛合金层。
在一种特定实施方案中，本发明的用于透明基材特别是用于玻璃板的高耐热性低发射率多层系统，其具有：下抗反射涂层，该涂层具有高折射层；基本上由ZnO组成的润湿层，该润湿层连接着以银为基础的功能层；在该功能层上面的阻隔层；上抗反射涂层，由一个层或几个部分层组成；以及覆盖涂层，其由一个层或几个部分层组成；在下抗反射底涂层中，在高折射层与润湿层之间设置了另外的金属氧化物层，其作为防散射层。位于高折射层与润湿层之间的防散射层是混合氧化物层，其厚度至少是0.5nm，由NiCrOx或InSnOx(ITO)构成。
在一种有利的实施方案中，本发明多层系统具有以下多层结构：玻璃/SnO2/TiO2/NiCrOx/ZnO:Al/Zn/Ag/TiAl(TiH1)/ZnO:Al/Si3N4/ZnSnSbOx/Zn2TiO4。
在另一种有利的实施方案中，
本发明多层系统具有以下多层结构：
玻璃/SnO2/TiO2/ITO/ZnO:Al/Zn/Ag/TiAl(TiH1)/ZnO:Al/Si3N4/ZnSnSbOx/Zn2TiO4。
下面将结合2个说明实施例更详细地描述本发明，它们与2个现有技术的对比例进行比较。鉴于本发明的布置特别地优化了光学和能量性质，故各个层品质的评估主要基于散射光、表面电阻和发射率的测定。因此，为评估该多层的性质，对涂布的窗板实施下面给出的测定和试验：
A.通过X-射线荧光分析测定银层厚度(d)；
B.采用散射光测定仪器(由Gardner公司提供)测定散射光(H)(％)；
C.采用散射光测定仪器(由Gardner公司提供)测定透射(T)(％)；
D.采用FPP 5000 Veeco Instr.仪器和SQOHM-1手动测定仪器测定表面电阻，Ω/□；
E.采用MK2测定仪器(由Sten
Figure A20068003058000051
公司提供)测定发射率(En)，％。
测定发射率之后，借助于表明电阻值通过公式E* n＝0.0106 x R(参看H.-J.
Figure A20068003058000052
：“Dünnfilmtechnologie auf Flachglas”，Verlag Karl Hofmann1999，144页)计算发射率的值，并将测定值En与计算值E* n进行比较。测量值En与计算值E* n之间的差值越小，多层系统的热稳定性越好。
就每一种测定而言，采用从4mm厚的涂布玻璃板中央部分切割的尺寸为40×50cm的样品。将样品在由EFKO公司生产的47067型增强炉中加热到720～730℃的温度，随后通过突然在空气中进行冷却实施热增强。所有样品均照此方式经受相同热应力。
还应当指出，本发明多层系统只有在对它沉积在其上的基材进行热处理(增强)之后，才在窗户的热绝缘、红外反射和光透射方面达到其最佳数值。防散射层在热处理期间也起到关键作用。然而，这里所描述的多层系统(也)可在商业上使用，只是热绝缘和光透射略嫌不足，甚至可不经热处理，并因此特别用于非-增强玻璃板上，或在合成材料玻璃板上，还有在薄膜上。然而，下面的说明实施例则全部关于多层系统在由热增强玻璃制成的玻璃板组成的基材上的应用。
对比例1
将对应于现有技术(DE 102 35 154 B4)的低发射率多层系统，采用反应磁控阴极喷射方法在连续涂布工业装置上，沉积在4mm厚浮法玻璃制成的玻璃板上，化学符号前面的数值表明每层以纳米为单位的厚度：玻璃/18SnO2/10TiO2/6ZnO:Al/1.5Zn/11.6Ag/2TiAl(TiH1)/5ZnO:Al/30Si3N4/3ZnSnSbOx/2Zn2 TiO4。
TiO2层是在Ar和O2混合物组成的工作气体中对2个由TiOx陶瓷组成的圆筒形靶喷射而被沉积的，O2的加入量为约3体积％。ZnO:Al层是通过对含2wt％Al的ZnAl的金属靶的喷射而被沉积的。薄Zn金属膜是在非反应性条件下从同样靶材料上被沉积的。位于银层上面的阻隔层是通过在Ar/H2(90/10，体积％)工作气体混合物中对金属靶反应性喷射被沉积的，靶含有64wt％Ti和36wt％Al。反应喷射期间，生成氢化钛，其氢化程度只能很困难地规定。如果结合是化学计量的，则1的值介于1～2之间。
上抗反射层是通过在Ar/N2工作气体混合物中对Si靶的反应性喷射被被沉积的。
从由含68wt％Zn、30wt％Sn和2wt％Sb的ZnSnSb合金组成的金属靶在Ar/O2工作气体中得到ZnSnSbOx下覆盖层，而上覆盖层(最后层)也是通过对由含73wt％Zn和27wt％Ti的ZnTi合金组成的金属靶反应性喷射被沉积的。
下面的数值是从对比例增强涂布的样品上测定的：
银层厚度：11.6nm
散射光H：0.70％
透射T：87.2％
表面电阻R：3.75Ω/□
测定的发射率En：9.65％
计算的发射率E* n：3.97％
En-E* n：5.68％
散射光的比例，等于0.7％，大大超过仍可容忍的极限0.5％。另外，发现在发射率测定值与计算值之间存在巨大差异。在卤素灯的斜射之下，看到一个薄(浑浊)膜。
对比例2
为继续比较，如对比例1所述的文献EP 1 538 131的多层系统，在TiO2层和ZnO层之间配备以SnO2防散射层。于是，该多层系统便具有了以下结构：
玻璃/18SnO2/10TiO2/5SnO2/6ZnO:Al/1.5Zn/11.6Ag/2TiAl(TiH1)/5ZnO:Al/30Si3N4/3ZnSnSbOx/2Zn2TiO4
对在与对比例1相同条件下热增强的样品进行测定，给出以下数值：
银层厚度：11.7nm
散射光H：                 0.50％
透射T：                   87.0％
表面电阻R：               3.1Ω/□
测定的发射率En：          7.2％
计算的发射率E* n：         3.3％
En-E* n：                  3.9％
由于配有SnO2防散射层，散射光的比例与上面对比例相比大大降低，但它依然有0.5％。还观察到在发射率的测定值与计算值之间很相近。在3.9％，该差值依旧比较大，应该得出以下结论，在增强操作期间银层仍然经历了相当程度的降解。
SnO2层的插入使多层系统整体上变得可塑性更强，这表现在较大的划伤敏感性和洗涤操作期间较大表面损伤倾向。
实施例1
在与对比例1和2使用的同样涂布装置上生产了一种根据本发明改良的多层系统，该系统具有以下结构：玻璃/18SnO2/10TiO2/2.5NiCrOx/6ZnO:Al/1.5Zn/11.6Ag/2TiAl(TiH1)/7ZnO:Al/30Si3N4/3ZnSnSbOx/2Zn2TiO4
相对于对比例2的改变在于，在TiO2层和ZnO层之间插入NiCrOx防散射层替代SnO2层。通过在Ar/O2气氛中，该工作气体的含氧量为约30体积％，以连续流模式对扁平金属靶喷射而沉积成低氧化态NiCrOx层。
样品按照与对比例的样品相同的方式进行增强处理。对增强、涂布的样品实施的测定给出以下数值：
银层厚度：                      11.5nm
散射光H：                       0.25％
透射T：                         89.1％
表面电阻R：                     3.68Ω/□
测定的发射率En：                4.3％(4.0～4.6％)
计算的发射率E* n：               3.9％
En-E* n：                        0.4％
因此，散射光的比例降低到对比例2的一半。同样，测定发射率与计算发射率之间的差值也变得相当小，从而可以得出结论，NiCrOx层的插入使银层在增强操作期间变得更稳定。
该多层系统在使用中的表现也大大得到改善，这表现在划伤显著降低的敏感性。即便当增强时间延长20％，也未观察到不利的效果。这表示多层系统的抗温度性得到进一步改善。该多层系统视觉上闪亮，即便在采用卤素灯斜射下也看不出(轻微浑浊)膜。
实施例2
在与前面的实施例使用的同样涂布装置上生产了一种根据本发明改良的多层系统，该系统具有以下结构：玻璃/18SnO2/6TiO2/2.5ITO/6ZnO:Al/1.5Zn/11.6Ag/2TiAl(TiH1)/7ZnO:Al/30Si3N4/3ZnSnSbOx/2Zn2TiO4
通过在不加O2的Ar气氛中，对陶瓷平面靶喷射而沉积ITO防散射层。
在与前面实施例的相同条件下热处理和增强处理后，对样品测定了以下数值：
银层厚度：                11.6nm
散射光H：                 0.25％
透射T：                   89.1％
表面电阻R：                  3.67Ω/□
测定的发射率En：             4.4％(4.2～4.6％)
计算的发射率E* n：            3.9％
En-E* n：                     0.5％
同样地，与对比例2的比较显示，本发明ITO防散射层给出好于SnO2防散射层的结果。

Claims (8)

1.一种用于透明基材，特别是用于玻璃板的高耐热性低发射率多层系统，其具有：下抗反射涂层，该涂层具有高折射层；基本上由ZnO组成的润湿层，该润湿层连接着以银为基础的功能层；在该功能层上面的阻隔层；上抗反射涂层，其由一个层或几个部分层组成；以及覆盖涂层，其由一个层或几个部分层组成；在下抗反射底涂层中，在高折射层与润湿层之间设置了另外的金属氧化物层，其作为防散射层，其特征在于，位于高折射层与润湿层之间的防散射层是混合氧化物层，其厚度至少是0.5nm，由NiCrOx或InSnOx(ITO)构成。
2.权利要求1的多层系统，其特征在于，高折射层由TiO2、Nb2O5或TiNbOx构成。
3.权利要求1或2的多层系统，其特征在于，高折射层直接配置在玻璃表面上。
4.权利要求1或2的多层系统，其特征在于，介电层，其折射指数n小于与它相邻的高折射层的折射指数，被配置于玻璃表面与高折射层之间。
5.前面权利要求的多层系统，其特征在于，被配置在玻璃表面与高折射层之间的介电层由SnO2、ZnO、SiO2或Si3N4构成。
6.前面权利要求任一项的多层系统，其特征在于，阻隔层是金属层或由50～80wt％Ti和20～50wt％Al组成的略微氢化的钛合金层。
7.权利要求1、2和4～6任一项的多层系统，其特征在于以下多层结构：玻璃/SnO2/TiO2/NiCrOx/ZnO:Al/Zn/Ag/TiAl(TiH1)/ZnO:Al/Si3N4/ZnSnSbOx/Zn2TiO4。
8.权利要求1、2和4～6任一项的多层系统，其特征在于以下多层结构：玻璃/SnO2/TiO2/ITO/ZnO:Al/Zn/Ag/TiAl(TiH1)/ZnO:Al/Si3N4/ZnSnSbOx/Zn2TiO4。
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DE102005039707A1 (de) 2007-03-01
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BRPI0614971A2 (pt) 2013-01-01
CA2620012C (fr) 2014-01-28
DE602006005683D1 (de) 2009-04-23

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Application publication date: 20081008