CN104105595A - 作为反射器的多层结构 - Google Patents

作为反射器的多层结构 Download PDF

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CN104105595A
CN104105595A CN201380009997.0A CN201380009997A CN104105595A CN 104105595 A CN104105595 A CN 104105595A CN 201380009997 A CN201380009997 A CN 201380009997A CN 104105595 A CN104105595 A CN 104105595A
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layer
sandwich construction
middle level
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thermoplastic
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CN104105595B (zh
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T.库尔曼
M.瓦格纳
R.奥瑟
T.G.戴维斯
I.奥西奥
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Covestro Deutschland AG
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    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
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Abstract

本发明涉及在CPV(聚光光伏)和CPS(聚光太阳能发电)领域用作反射镜/反射器的多层结构。所述多层结构包含基体层、阻挡层、金属反射层、氧化物层和一个其它层，所述其它层可以是等离子体聚合物层或高折射金属氧化物层。

Description

作为反射器的多层结构
本发明涉及在CPV(聚光光伏)和CPS(聚光太阳能发电)领域用作反射镜/反射器的多层结构。所述多层结构包含基体层、阻挡层、金属反射层、氧化物层和一个其它层，所述其它层可以是等离子体聚合物层或高折射金属氧化物层。
用于CPV和CPS领域中的银反射镜是已知的。
WO 2000007818描述了基于带有直接施加在其上的银层的聚合物基体的银反射镜，所述银进而覆盖有直接施加于其上并坚固地与之粘合的聚合物保护层。UV吸收聚合物膜施加在此聚合物层上。
US 6078425描述了含有铝和银反射层的多层反射镜，其中镍和/或铬合金或氮化物的粘合层沉积在所述铝的表面上。所述银层受镍和/铬合金或氮化物形成的层和一个或多个金属氧化物层的保护。
根据Society of Vacuum Coaters (2009)，52版，473-477，基于由金属层(Al或Cu)、银反射层、氧化铝透明保护层或带有施加于其上的SiO2的氮化硅层和氧化钽层构成的已知体系，替换所述复杂的保护层体系以便在短程金属化装置内进行大量生产。据报道生产的层状结构依然具有足够的反射性和耐候性。
因此，Society of Vacuum Coaters (2009)，52版，473-477公开了具有增加的反射性和耐候性的特殊的多层结构。其中描述了层状结构，其具有塑料基体、金属层、施加于其上的银反射器和等离子体硅氧烷面漆。然而，描述的所述结构不符合必要的需要。
在Concentrating Photovoltaic Conference 7 (CPV 7)，Las Vegas，2011年4月中已知需要提供用于CPV应用的耐久性长的高反射的银反射镜。在此情况下提出了通用形式的各种解决方案。尤其是，提出了具有下面通用结构的体系：基体、金属、银反射器、金属氧化物、HMDSO。
在SVC/Society of Vacuum Coaters 2009，Optics O21中，作为制备反射性、耐腐蚀的金属多层体系的简单方法描述了等离子体涂敷，并进行了实验。据描述，使用此方法目前为止在上面描述的短程涂敷中尚未使用氧化铝保护层。
在Surface and Coatings Technology 111 (1999) 278-296中，描述了由等离子体预处理、溅射和等离子体聚合组合所得的铝反射镜用于制造汽车灯。
然而，上面提及的体系的性能特征不足以用于CPV和CSP领域中的反射器，尤其是关于在户外使用时的寿命期间保持高的反射率。特别地，对于由于风化作用增加的腐蚀造成的对反射率的不利影响对于商业用途来说依然没有令人满意地解决。另外，应当可以简单且成本有效地大量生产这些多层体系。
因此，本发明的目的是提供一种多层体系，其在整个寿命周期内恒定不变地提供高的反射率，其中可以通过简单且成本有效的方法生产该类多层体。另外，所述多层体系应当具有高的尺寸稳定性、低的开裂趋势和低的表面粗糙度，由此满足DIN EN 62108关于气候变化稳定性的要求 (第10.6、10.7和10.8章)。
所述目的通过包含如下5个层的多层结构得以实现：
层A：基体层，选自热塑性塑料、金属或玻璃；
层B：阻挡层，选自钛或贵金属族，其中优选贵金属是金、钯、铂、钒和钽。在玻璃作为所述基体层的情况下，所述阻挡层也可以另外由铬或铬与Co、Mo、Ni和/或Fe的合金制成；
层C：金属反射层，优选由银或银合金以及铝组成，其中所述银合金含有小于10重量%的金、铂、钯和/或钛；
层D：氧化物层，选自氧化铝(AlOx)、二氧化钛、SiO2、Ta2O5、ZrO2、Nb2O5和HfO；
层E：
a) 等离子体聚合物层(防腐蚀层)，其由硅氧烷前体沉积而成，优选的实例是六甲基二硅氧烷(HMDSO)、八甲基环四硅氧烷(OMCTS)、八甲基三硅氧烷(OMTS)、四乙基正硅烷(TEOS)和四甲基二硅氧烷(TMDSO)、十甲基环五硅氧烷(DMCPS)、六甲基环三硅氧烷(HMCTS)、三甲氧基甲基硅烷(TMOMS)和四甲基环四硅氧烷(TMCTS)；HMDSO是特别优选的；或者，在层D由氧化铝或SiO2组成的情况下，层E是
b) 高折射金属氧化物层，其中所述金属氧化物可以选自二氧化钛、SiO2、Ta2O5、ZrO2、Nb2O5和HfO，并且可以任选地施加根据层E(a)的另一个层，即：等离子体聚合物层。
所述实例表明：此多层结构具有高的尺寸稳定性、低的开裂趋势和低的表面粗糙度的所要求的性能特点，由此满足DIN EN 62108关于气候变化稳定性的要求 (第10.6、10.7和10.8章)。
层A：
层A选自太热塑性塑料、金属或玻璃。
用于所述基体层的优选的热塑性塑料是聚碳酸酯、聚苯乙烯、苯乙烯共聚物、芳族聚酯如聚对苯二甲酸乙二醇酯(PET)、PET/环己烷二甲醇共聚物(PETG)、聚萘二甲酸乙二醇酯(PEN)、聚对苯二甲酸丁二醇酯(PBT)、环状聚烯烃、聚-或共聚丙烯酸酯和聚-或共聚甲基丙烯酸酯，例如聚-或共聚甲基丙烯酸甲酯(如PMMA)以及与苯乙烯的共聚物，例如透明的聚苯乙烯/丙烯腈(PSAN)，热塑性聚氨酯，基于环状烯烃的聚合物(例如TOPAS®，购自Ticona的商品)，与烯烃共聚物或接枝聚合物的聚碳酸酯共混物，例如苯乙烯/丙烯腈共聚物。聚碳酸酯、PET或PETG是特别优选的。特别地，所述基体层由聚碳酸酯组成。
根据本发明，聚碳酸酯是均聚碳酸酯、共聚碳酸酯和聚酯碳酸酯，例如EP-A 1,657,281中的那些。
例如通过相界面法，任选使用链终止剂，例如单酚，和任选地使用三官能或大于三官能的支化剂，例如三酚或四酚，通过使二酚与碳酰卤，优选光气，和/或与芳族二羧酰二卤，优选苯二羧酰二卤进行反应来制备芳族聚碳酸酯。它们也可以通过二酚与例如碳酸二苯基酯的反应以熔融聚合法制备。
用于制备芳族聚碳酸酯和/或芳族聚酯碳酸酯的二酚优选是式(I)的那些
其中
A是单键、C1-C5-亚烷基、C2-C5-烷叉、C5-C6-环烷叉、-O-、SO、-CO-、-S-、-SO2-、C6-C12-亚芳基，在其上可以稠合其它的任选地含有杂原子的芳族环，或式(II)或(III)的基团
B分别为C1-C12-烷基优选甲基，或卤素优选氯和/或溴，
x分别相互独立地为0、1或2，
p是1或0，
R5和R6对于每个X1是可以单独选择的并且相互独立地为氢或C1-C6-烷基, 优选氢、甲基或乙基，
X1是碳，和
m是4-7的整数，优选为4或5，条件是R5和R6在至少一个X1原子上同时为烷基。
适合用于制备聚碳酸酯的二酚例如有：氢醌、间苯二酚、二羟基联苯、双-(羟基苯基)链烷烃、双(羟基苯基)环烷烃、双-(羟基苯基)硫醚类、双-(羟基苯基)醚类、双-(羟基苯基)酮类、双-(羟基苯基)砜类、双-(羟基苯基)亚砜类、α,α'-双(羟基苯基)二异丙基苯、由靛红衍生物或酚酞衍生物衍生的苯并[c]吡咯酮，和其环上烷基化和环上卤代的化合物。
优选的二酚是4,4'-二羟基联苯、2,2-双-(4-羟基苯基)丙烷、2,4-双-(4-羟基苯基)-2-甲基丁烷、1,1-双-(4-羟基苯基)-对二异丙苯、2,2-双-(3-甲基-4-羟基苯基)丙烷、2,2-双-(3-氯-4-羟基苯基)丙烷、双-(3,5-二甲基-4-羟基苯基)甲烷、2,2-双-(3,5-二甲基-4-羟基苯基)丙烷、双-(3,5-二甲基-4-羟基苯基)砜、2,4-双-(3,5-二甲基-4-羟基苯基)-2-甲基丁烷、1,1-双-(3,5-二甲基-4-羟基苯基)-对二异丙苯、2,2-双-(3,5-二氯-4-羟基苯基)丙烷、2,2-双-(3,5-二溴-4-羟基苯基)丙烷、1,1-双-(4-羟基苯基)- 3,3,5-三甲基环己烷和2-烃基-3,3-双(4-羟基芳基)苯并[c]吡咯酮以及N-苯基靛红和苯酚的反应产物。
特别优选的二酚是：2,2-双-(4-羟基苯基)-丙烷、2,2-双-(3,5-二甲基-4-羟苯基)丙烷、2,2-双-(3,5-二氯-4-羟基苯基)丙烷、2,2-双-(3,5-二溴-4-羟基苯基)丙烷、1,1-双-(4-羟基苯基)环己烷和1,1-双-(4-羟基苯基)-3,3,5-三甲基环己烷。
在均聚碳酸酯的情况下，仅使用一种二酚；在共聚碳酸酯的情况下，则使用几种二酚。合适的碳酸衍生物的实例是光气或碳酸二苯酯。
在聚碳酸酯的制备中可以使用的适合的链终止剂是一元酚和一元羧酸。适合的一元酚是苯酚本身，烷基酚如甲酚、对-叔丁基苯酚、枯基苯酚、对-正辛基苯酚、对-异辛基苯酚、对-正壬基苯酚和对-异壬基苯酚，卤酚如对-氯苯酚、2,4-二氯苯酚、对-溴苯酚和2,4,6-三溴苯酚、2,4,6-三碘苯酚、对-碘苯酚，和它们的混合物。优选的链终止剂是苯酚、枯基酚和/或对-叔丁基苯酚。
在本发明范围内，特别优选的聚碳酸酯是基于双酚A的均聚碳酸酯和基于选自双酚A、1,1-双(4-羟基苯基)-3,3,5-三甲基环己烷、2-烃基-3,3-双(4-羟基芳基)苯并[c]吡咯酮和N-苯基靛红与苯酚的反应产物中的至少一种的单体的共聚碳酸酯。所述聚碳酸酯可以是以已知方式地线性的或支化的。共聚单体的比例基于双酚A计通常为最多60重量%，优选最多50重量%和特别优选3-30重量%。也可以使用均聚碳酸酯和共聚碳酸酯的混合物。
含有2-烃基-3,3-双(4-羟基芳基)苯并[c]吡咯酮作为单体的聚碳酸酯和共聚碳酸酯尤其由EP 1 582 549 A1已知。含有基于N-苯基靛红和苯酚的反应产物的双酚单体的聚碳酸酯和共聚碳酸酯描述于例如WO 2008/037364 A1中。
该热塑性芳族聚碳酸酯具有10,000至80,000克/摩尔，优选14,000至32,000克/摩尔和特别优选18,000至32,000克/摩尔的平均分子量(重均Mw，通过使用聚碳酸酯标准物的GPC(凝胶渗透色谱法)测得)。在聚碳酸酯注射模塑成型体的情况下，优选的平均分子量为20,000-29,000 g/mol。在聚碳酸酯成型体挤出的情况下，优选的平均分子量为25,000-32,000 g/mol。
所述聚碳酸酯也可以含有填料。合适的填料是玻璃球、空心玻璃球、玻璃片、炭黑、石墨、碳纳米管、石英、滑石、云母、硅酸盐、叠氮化物、硅灰石和热解或沉淀硅酸，其中硅酸具有至少50 m2/g的BET表面积(根据DIN 66131/2)。
优选的纤维状填料是金属纤维、碳纤维、塑料纤维、玻璃纤维或磨砂玻璃纤维，其中玻璃纤维或磨砂玻璃纤维是特别优选的。优选的玻璃纤维还有以实施方式连续纤维（粗纱）、长玻璃纤维和短切玻璃纤维使用的那些，其由M-、E-、A-、S-、R-或C-玻璃制成的，其中E-、A-或C-玻璃是特别优选的。
所述纤维的直径优选为5-25μm，进一步优选6-20μm 和非常特别优选为7-15μm。所述长玻璃纤维具有的长度优选为5-50 mm，特别优选为5-30 mm，非常特别优选为6-15 mm和尤其是7-12 mm；它们描述于例如WO-A 2006/040087中。所述短切玻璃纤维当占所述玻璃纤维的至少70重量%时优选具有的长度大于60μm。
其它无机纤维是无机颗粒，其颗粒形状选自球形/立方形、片状/圆盘状和平板状几何形状。特别合适的无机填料是具有球形或平板状的那些，优选为具有大的外表面积和/或内表面积的细分和/或多孔形式的那些。这些优选的是热惰性的无机材料，其特别是基于氮化物，例如氮化硼；或者是氧化物或混合氧化物，如氧化铈、氧化铝；碳化物，如碳化钨、碳化硅或碳化硼；粉末石英，如石英粉、无定形SiO2；粉砂；玻璃颗粒，如玻璃粉，特别是玻璃球；硅酸盐或硅铝酸盐；石墨，特别是高纯度合成石墨。石英和滑石是特别优选的，石英是最优选的(球形颗粒形状)。这些填料特征在于平均直径d50%为0.1-10 µm，优选为0.2-8.0 µm并特别优选为0.5-5 µm。
所述硅酸盐特征在于平均直径d50%为2-10 µm，优选为2.5-8.0µm，特别优选为3-5µm并尤其是3µm，其中上部直径d95%相应地优选为6-34µm，特别优选为6.5-25.0µm，非常特别优选为7-15 µm和尤其是10µm。根据ISO 9277通过氮吸附测定，所述硅酸盐具有的BET比表面积优选为0.4-8.0m2/g，更优选为2-6m2/g并非常特别优选为4.4-5.0m2/g。
特别优选的硅酸盐含有至多仅仅3重量%的次要成分，优选为下面的比例：
Al2O3 < 2.0重量%，
Fe2O3 < 0.05重量%，
(CaO + MgO) < 0.1重量%，
(Na2O + K2O) < 0.1重量%，分别基于硅酸盐的总重量计。
另一个有利的实施方案使用细磨类型形式的硅灰石或滑石，其中平均粒径d50为<10µm，优选为< 5µm，特别优选为<2µm和非常特别优选为<1.5µm。粒度分布通过风选测定。
所述硅酸盐可以具有有机硅化合物涂层，其中优选使用环氧基硅烷、甲基硅氧烷和甲基丙烯酰基硅烷浆料。特别优选环氧基硅烷浆料。
所述填料可以以基于聚碳酸酯的量计最高达40重量%的量加入。优选的量为2.0-40.0重量%，优选3.0-30.0重量%，特别优选5.0-20.0重量%和非常特别优选7.0-14.0重量%。
用于聚碳酸酯的合适的共混组分是乙烯基单体在接枝基础如二烯橡胶或丙烯酸酯橡胶上的接枝聚合物。接枝聚合物B优选B.1在B.2上接枝制成：
B.1 5-95重量%，优选30-90重量%的至少一种乙烯基单体，
B.2 95-5重量%，优选70-10重量%的一种或多种接枝基础，具有的玻璃化转变温度为<10℃，优选< 0℃和特别优选<–20℃。
接枝基础B.2通常具有的平均粒径(d50值)为0.05-10μm，优选0.1-5μm和更优选0.2-1μm。
单体B.1优选是B.1.1和B.1.2的混合物：
B.1.1 50-99重量份的乙烯基芳族化合物和/或环取代的乙烯基芳族化合物(如苯乙烯、α-甲基苯乙烯、对甲基苯乙烯、对氯苯乙烯)和/或甲基丙烯酸(C1-C8)烷基酯(如甲基丙烯酸甲酯、甲基丙烯酸乙酯)，和
B.1.2 1-50重量份乙烯基氰化物(不饱和腈，如丙烯腈和甲基丙烯腈)和/或(甲基)丙烯酸(C1-C8)烷基酯(如甲基丙烯酸甲酯、丙烯酸正丁酯、丙烯酸叔丁酯)和/或不饱和羧酸的衍生物(如酸酐和酰亚胺)，例如马来酸酐和N-苯基马来酰亚胺。
优选的单体B.1.1选自单体苯乙烯、α-甲基苯乙烯和甲基丙烯酸甲酯中的至少一种，优选的单体B.1.2选自单体丙烯腈、马来酸酐和甲基丙烯酸甲酯中的至少一种。特别优选的单体对于B.1.1是苯乙烯和对于B.1.2是丙烯腈。
用于接枝聚合物B的合适的接枝基础B.2的实例是二烯橡胶、EP(D)M橡胶（即基于乙烯/丙烯和任选的二烯的橡胶）、丙烯酸酯橡胶、聚氨酯橡胶、硅酮橡胶、氯丁二烯和乙烯/乙酸乙烯酯橡胶。
优选的接枝基础B.2是例如基于丁二烯和异戊二烯的二烯橡胶，或二烯橡胶的混合物或二烯橡胶的共聚物或它们与其它可共聚单体(例如根据B.1.1和B.1.2)的混合物，条件是组分B.2的玻璃化转变温度低于<10℃，优选<0℃，特别优选<-10℃。纯的聚丁二烯橡胶是特别优选的。
特别优选聚合物B的实例是ABS聚合物(乳液-、本体-和悬浮-ABS)，例如在DE-OS 2 035 390 (= USPS 3 644 574)或 DE-OS 2 248 242 (= GB-PS 1 409 275)中和Ullmanns, Enzyklopädie der Technischen Chemie, 卷19(1980), 第280页及以后中所描述的那些。所述接枝基础B.2的凝胶含量为至少30重量%，优选至少40重量%(在甲苯中测量)。
通过自由基聚合，例如通过乳液-、悬浮-、溶液-或本体-聚合，优选通过乳液或本体聚合制备接枝共聚物B。
因为已知在接枝反应中接枝单体不是必然完全接枝在所述接枝基础上，所以接枝聚合物Ｂ根据本发明应当理解为是指包括在所述接枝基础存在下由接枝单体(共)聚合产生的以及在后处理过程中与所述接枝聚合物B一起获得的产物。
所述聚合物组合物也可以以常规用于所讨论的热塑性塑料的量任选地含有EP-A 0 839 623、WO-A 96/15102、EP-A 0 500 496 或“Plastics Additives Handbook”, Hans Zweifel, 第5版，2000, Hanser Verlag, Munich描述的其它常规的聚合物添加剂，例如抗氧化剂、热稳定剂、脱模剂、光学增亮剂、UV吸收剂和光散射剂。
合适的UV稳定剂是苯并三唑、三嗪、二苯甲酮和/或芳基化的氰基丙烯酸酯。特别合适的紫外线吸收剂是羟基苯并三唑类，例如2-(3',5'-双-(1,1-二甲基苄基)-2'-羟基苯基)-苯并三唑(Tinuvin® 234, Ciba Spezialitätenchemie, Basel)、2-(2'-羟基-5'-(叔辛基)-苯基)-苯并三唑(Tinuvin® 329, Ciba Spezialitätenchemie, Basel)、2-(2'-羟基-3'-(2-丁基)-5'-(叔丁基)-苯基)-苯并三唑(Tinuvin® 350, Ciba Spezialitätenchemie, Basel)、双-(3-(2H-苯并三唑基)-2-羟基-5-叔辛基)甲烷(Tinuvin® 360, Ciba Spezialitätenchemie, Basel)、(2-(4,6-二苯基-1,3,5-三嗪-2-基)-5-(己基氧基)-苯酚(Tinuvin® 1577, Ciba Spezialitätenchemie, Basel)和二苯甲酮类，例如2,4-二羟基二苯甲酮(Chimassorb® 22, Ciba Spezialitätenchemie, Basel)和2-羟基-4-(辛基氧基)-二苯甲酮(Chimassorb® 81, Ciba, Basel), 2-丙酸、2-氰基-3,3-二苯基-, 2,2-双[[(2-氰基-1-氧代-3,3-二苯基-2-丙烯基)氧基]-甲基]-1,3-丙二基酯(9CI) (Uvinul® 3030, BASF AG Ludwigshafen)、2-[2-羟基-4-(2-乙基己基)氧基]苯基-4,6-二(4-苯基)苯基-1,3,5-三嗪(CGX UVA 006, Ciba Spezialitätenchemie, Basel)或四乙基-2,2'-(1,4-亚苯基二亚甲基)-双丙二酸酯(Hostavin® B-Cap, Clariant AG)。
所述聚合物组合物通常可以含有基于总的组合物计0-5重量%，优选0.1-2.5重量%的量的UV吸收剂。
所述聚合物组合物通过常用的引入法制备，其中将各成分集合、混合和均化；所述均化特别优选在熔体中在剪切力作用下进行。任选地，在熔体均化之前的集合与混合使用粉末预混物进行。
所述基体材料可以采用薄膜或片材的形式。可以使所述薄膜变形和与选自上面提及的热塑性塑料中的另一热塑性塑料一起反向注射模塑(薄膜插入模塑(FIM))。所述片材可以热成型、通过包模成型进行加工或冷弯曲。成型也可以通过注射模塑法进行。这些方法是本领域技术人员已知的。
所述基体层的层厚度必须确保所述组件足够的刚性。
在薄膜的情况下，基体层A可以通过反向注射模塑进行增强以确保足够的刚性。
层A的总厚度(即包括可能的反向注射模塑件)通常为1μm –10mm。特别优选地，层A的厚度为1mm–10mm、1mm–5mm或 2 mm–4 mm。特别地，所述厚度数据指的是当使用聚碳酸酯作为基体材料时总的基体厚度，包括可能的反向注射模塑件。
在PET的情况下，所述层厚度优选为10μm–100μm(PET)，PC膜的厚度优选为100μm–1mm(PC膜)，其中可以通过反向注射模塑件增强这些热塑性塑料。
在金属基体的情况下，所述层厚度通常为300μm–750μm。在玻璃基体的情况下，所述层厚度通常为750μm–3mm，优选为800μm–2 mm。
层B：
层B选自上面提及的金属。层B优选不含铜或含铜化合物或含铜合金。
层B的厚度通常为40nm–250nm，优选55nm–200nm和尤其是为80nm–130nm。
使用钛时特别优选的层厚度为105nm–120nm。
层C：
层C的厚度通常为80nm–250nm，优选90nm–160nm和特别优选为100nm–130nm。
在银的情况下，使用高纯度银。市购可得的产品由Heraeus Precious Metals(例如：Ag靶，纯度3N7)或Umicore可获得。
层D：
层D的厚度通常为80nm–250nm，优选90nm–160nm，特别优选为90nm–130nm和非常特别优选为90nm–110nm。
层E：
层E的厚度通常为1nm–200nm，优选10nm–150nm，特别优选为20nm–100nm和非常特别优选为30nm–50nm。
施加各个层：
层B和C都是通过气化渗镀或溅射施加。
层D用氧气作为反应性气体通过反应性气化渗镀或反应性溅射施加。这些方法是通常已知的且描述于例如Vakuumbeschichtung，卷1-5，Ed.Hartmut Frey，VDI Verlag, 1995。
金属可以通过各种方法施加到聚合物上，例如由气化渗镀或溅射。所述方法例如更详细地描述于“Vakuumbeschichtung 卷1-5", H. Frey, VDI-Verlag Düsseldorf 1995或"Oberflächen- und Dünnschicht-Technologie”第1部分，R.A. Haefer, Springer Verlag 1987。
为了达到更好的金属粘附性和为了清洁基体表面，通常使所述基体经历等离子体预处理。等离子体预处理可以主要改变聚合物的表面性能。例如Friedrich等在Metallized plastics 5 & 6: Fundamental and applied aspects和H. Grünwald等在Surface and Coatings Technology 111 (1999) 287-296中描述了这些方法。
层E通过PECVD(等离子体增强的化学蒸气沉积)或等离子体聚合法施加。其中主要基于硅氧烷的低沸点前体被气化成等离子体并由此活化，使得它们可以形成薄膜。所述方法尤其描述于Surface and Coatings Technology 111 (1999) 287-296中。
可以施加其它的功能层，例如用于抵抗机械应力的层和/或基于高折射金属氧化物(例如TiO2)的反射增强层。这样的层描述在例如WO 2010/127805和WO 2010/085909中。
根据本发明的多层结构可以用作光伏模块(聚光光伏)、太阳能模块(聚光太阳能发电)和照明系统的反射器、作为住宅领域和车辆领域(例如航空器和轨道车辆、公共汽车、公用车辆和机动车)中的反射镜和作为光导系统中的反射器。因此，本发明还提供了包含根据本发明的多层结构的光伏模块、太阳能模块和照明系统。
本发明通过下面的实施例更详细地进行说明，但不意味着限制。根据本发明的实施例仅给出本发明优选的实施方案。
实施例：
层A的制备
基于双酚A的聚碳酸酯片材(105 x 150 x 3.2 mm)：
PC-1：Makrolon® 2407，Bayer MaterialScience AG, Leverkusend，德国，其中熔体体积流速(MVR)为19 cm3/10 分钟，根据ISO 1133在300和1.2 kg下测量。
PC-2：Makrolon® 2808，Bayer MaterialScience AG, Leverkusend，德国，其中熔体体积流速(MVR)为9 cm3/10 分钟，根据ISO 1133在300和1.2 kg下测量。
片材的制备：
制成带有侧浇口的尺寸150 x 105 x 3.2 mm的长方形注射模塑片材。物料温度为300–330℃和模具温度为100℃。在加工之前，将每种粒料在真空干燥箱中在120℃下干燥5小时。
层A的粗糙度的测定
由于为聚光光学，所以整个系统的效率大大取决于散射光。使发生散射的光最小化的前体条件是光滑的基体表面。测定在注射模塑中模塑成型的表面的粗糙度。使用Ra(平均粗糙度)作为所述粗糙度的量度。使用下面的方法用于测量在未涂敷的片材上使用不同大小的测量区域的值，以便能够确立在较大面积上的粗糙度：
● AFM (原子力显微术)：
○ 所检查的测量区域大小：5 µm x 5 µm
○ 所检查的测量区域大小：20 µm x 20 µm
● WLI (白光干扰测定法)：
○ 所检查的测量区域大小：100 µm x 100 µm。
所述粗糙度Ra在5nm以下，因此所呈现的表面是非常光滑的。
层B：
使用下面的金属作为层B：
钛(根据本发明)，或者铜和铝(二者都是对比例)。
进行实验以便测定用于制备层B的特定金属的适合性。类似于对实施例1的描述制备在下面表1中描述的多层结构。
表 1：
为了评价耐腐蚀性，将所述样品在45℃和100%相对湿度下储存10天，然后目测进行光学评价。
结果：
· 样品A：银层变得发白并部分剥离
· 样品B：无可见缺陷
· 样品C：银层变色为金色，银与铜相互扩散。
评价表明：由于所述令人惊讶地差的耐腐蚀性，所以铜不适合作为用于层B的材料。因此，在本发明范围内没有对含铜的多层体系进行进一步的实验。
实施例1：多层结构(根据本发明的实施例)
PC片材(PC-1)如下面描述进行涂敷。制备下面的层状结构：
3.2 mm基体\\110 nm Ti\\120 nm Ag\\100 nm AlOx\\40 nm HMDSO。
制备方法：
1. 将所述PC片材转移到真空室中，所述真空室抽真空低至p < 2∙10– 5 mbar。
2. 等离子体预处理：将所述PC片材在500 W和0.1 mbar Ar下在中频等离子体中(40 kHz)预处理1分钟。
3. 层B：通过DC溅射沉积所述钛层。使用的涂敷源为来自Thin Film Consulting的直径200 mm的ION`X-8″HV圆形平面磁控管，所述涂敷源通过来自Advanced Energy的“Pinnacle™ Plus+ 5 kW”发生器进行工作。首先，所述靶(这里：钛)在封闭的遮掩物（Blende）下预溅射1分钟，并接着将所述钛层在3分钟40秒内在2000W和压力p = 5∙10– 3 mbar下在打开遮蔽物的情况下沉积在PC片材上。
4. 层C：通过DC溅射沉积所述银层。使用的涂敷源为来自Thin Film Consulting的直径200 mm的ION`X-8″HV圆形平面磁控管，所述涂敷源通过来自Advanced Energy的“Pinnacle™ Plus+ 5 kW”发生器进行工作。首先，所述靶(这里：银)在封闭的遮掩物下预溅射1分钟，并接着将所述银层在51秒内在2000W和压力p = 5∙10– 3 mbar下在打开遮蔽物的情况下沉积在所述钛层上。
接着将所述涂敷的PC片材从涂敷设备中移出并将涂覆设备准备用于后面的层。
5. 将所述涂敷的PC片材返回到真空室中，所述真空室抽真空低至p < 2∙10– 5 mbar。
6. 等离子体预处理：将所述涂敷的PC片材在500 W和0.1 mbar Ar下在中频等离子体中(40 kHz)预处理1分钟。
7. 层D：在脉冲频率150kHz通过脉冲DC反应性溅射沉积所述AlOx层。使用的涂敷源为来自Thin Film Consulting的直径200 mm的ION`X-8″HV圆形平面磁控管，所述涂敷源通过来自Advanced Energy的“Pinnacle™ Plus+ 5 kW”发生器进行工作。首先，所述靶(这里：铝)在封闭的遮掩物下预溅射1分钟，并接着将所述 AlOx层在4分钟内在340V在电压调节模式和在总压力p = 5∙10– 3 mbar下在打开遮蔽物的情况下沉积在所述银层上。O2/Ar比率调节为8%。
8. 层E：通过等离子体聚合将HMDSO(六甲基二硅氧烷)施加到AlOx层上作为另外的保护层。在35秒内在初始压力p = 0.038 mbar、流速90 sccm HMDSO和中频功率(40 kHz)1500 W下施加所述层。使用的所述源为片材间距为大约200 mm的平行反应器单元，其中所述片材位于中间。所述源通过Advanced Energy PEII (5 kW)（包括LMII高压变压器）进行操作。
在所有涂敷步骤中，所述片材在所述涂敷源上以大约20rpm旋转以便增加涂层的均匀性。
实施例2：不用HMDSO的对比例
将所述PC片材(PC-1)类似于实施例1用下面的层状结构涂敷，然而其中不施加HMDSO涂层：
3.2 mm基体\\110 nm Ti\\120 nm Ag\\100 nm AlOx
在所有涂敷步骤中，所述样品/片材在所述源上以大约20rpm旋转以便增加涂层的均匀性。
实施例3：对比例
在层C中用铝代替银。
PC片材(PC-1)如下进行涂敷：
3.2 mm基体\\大约100 nm Al\\大约40 nm HMDSO。
制备方法：
1. 将所述PC片材转移到真空室中，所述真空室抽真空低至p < 2∙10– 5 mbar。
2. 等离子体预处理：将所述PC片材在500 W和0.1 mbar Ar下在中频等离子体中(40 kHz)预处理1分钟。
3. 层C：通过DC溅射沉积所述铝层。使用的涂敷源为来自Thin Film Consulting的直径200 mm的ION`X-8″HV圆形平面磁控管，所述涂敷源通过来自Advanced Energy的“Pinnacle™ Plus+ 5 kW”发生器进行工作。首先，所述靶(这里：铝)在封闭的遮掩物下预溅射2分钟，并接着将所述Al层在150秒内在2000W和压力p = 5∙10– 3 mbar下在打开遮蔽物的情况下沉积。
4. 层E：通过等离子体聚合将HMDSO(六甲基二硅氧烷)施加到所述Al层上作为保护层。在35秒内在初始压力p = 0.038 mbar、流速90 sccm HMDSO和中频功率(40 kHz)1500 W下施加所述层。使用的所述源为片材间距为大约200 mm的平行反应器单元，其中所述样品/片材位于中间。所述涂敷源通过Advanced Energy PEII (5 kW)（包括LMII高压变压器）进行操作。
在所有涂敷步骤中，所述样品/片材在所述涂敷源上以大约20rpm旋转以便增加涂层的均匀性。
层厚度的调节
层厚度通过首先校准工艺参数进行调节。为此，在规定的工艺参数下将不同的层厚度沉积在显微镜载片上，所述载片中间带有胶带以产生台阶。在沉积各个层之后，除去胶带并用Tencor Instruments的KLA-Tencor Alpha-Step 500表面轮廓仪测定形成的台阶高度。
这样能够测定用于制备需要的目标层厚度必须调节的工艺参数。
成品部件上的层厚度的测量
所述层厚度可以在成品部件上通过TOF-SIMS(时间飞行–二次离子质谱法)或通过XPS(X-射线光子光谱法)结合TEM(透射电子显微术)进行测定。
风化结果
表 2：试验和评价方法：
试验 条件 时间(h) 评价
气候变化试验(DIN EN 62108 10.6 & 10.8) 在–40℃至110℃100次循环(每天14次循环)，接着进行20次湿度冷冻试验循环(20小时在85℃/85%相对湿度，接着进行4小时冷却到–40℃，然后再加热到85℃/85%相对湿度) 大约650小时 测定RI
氙气试验 0.75 W/m2/nm，在340 nm，Boro-Boro滤波器，黑色面板温度70℃，50%相对湿度，无雨 1000小时 测定RI
湿热试验(DIN EN 62108 10.7) 85℃，85%相对湿度 1000小时 测定RI
干热试验 在循环风干室中在125℃ 1000小时 测定RI
RI(反射系数)的测定：
1. 以Spectralon 标准校准的Perkin Elmer Lambda 900分光计在λ = 200-1100 nm范围测定总反射率(R总)和漫反射率(R漫反射)
2. 镜面反射的计算：R镜面 = R总–R漫反射
3. RIi的计算
4. 其中当i = 1, 2时， RI = 最小 (RIi)
EQEi(λ)(外量子效率)：例如Spectrolab C1MJ
SP(λ) = 根据ASTM G173-03的太阳光谱。
表 3：将以下样品进行风化：
表 4：镜面反射率和RI–初始值：
表 5：风化后的RI：
实施例2和3的层(对比例)显示了令人不满意的风化行为，但是实施例1的层(根据本发明)符合满足对于高折射率的耐久性的必要需求的要求。

Claims (16)

1.多层结构，包含如下5个层：
层A：基体层，选自热塑性塑料、金属或玻璃；
层B：阻挡层，选自钛或贵金属族，其中优选贵金属是金、钯、铂、钒和钽，其中在玻璃作为所述基体层的情况下，所述阻挡层也可以另外由铬或铬与Co、Mo、Ni和/或Fe的合金制成；
层C：金属反射层；
层D：氧化物层，选自氧化铝(AlOx)、二氧化钛、SiO2、Ta2O5、ZrO2、Nb2O5和HfO；
层E：
a) 等离子体聚合物层(防腐蚀层)，其由选自如下的硅氧烷前体沉积而成：六甲基二硅氧烷(HMDSO)、八甲基环四硅氧烷(OMCTS)、八甲基三硅氧烷(OMTS)、四乙基正硅烷(TEOS)和四甲基二硅氧烷(TMDSO)、十甲基环五硅氧烷(DMCPS)、六甲基环三硅氧烷(HMCTS)、三甲氧基甲基硅烷(TMOMS)和四甲基环四硅氧烷(TMCTS)；
或者，
在层D由氧化铝或SiO2组成的情况下，
b) 高折射金属氧化物层，其中所述金属氧化物可以选自二氧化钛、Ta2O5、ZrO2、Nb2O5和HfO，并且可以任选地施加根据层E(a)的另一个层，等离子体聚合物层。
2.根据权利要求1的多层结构，其中所述热塑性塑料选自下组中的至少一种：聚碳酸酯、聚苯乙烯、苯乙烯共聚物、芳族聚酯、环状聚烯烃、聚-或共聚丙烯酸酯和聚-或共聚甲基丙烯酸酯、与苯乙烯的共聚物、热塑性聚氨酯、基于环状烯烃的聚合物和与烯烃共聚物或接枝聚合物例如苯乙烯/丙烯腈共聚物的聚碳酸酯共混物。
3.根据权利要求1的多层结构，其中层B由钛组成。
4.根据权利要求1的多层结构，其中层C由银或银合金以及铝组成，其中所述银合金含有小于10重量%的金、铂、钯和/或钛。
5.根据权利要求4的多层结构，其中层C由银组成。
6.根据权利要求1的多层结构，其中层D由氧化铝(AlOx)或二氧化钛组成。
7.根据权利要求1的多层结构，其中层E是六甲基二硅氧烷。
8.根据权利要求1的多层结构，其中各个层的层厚度如下：
层A的总厚度：在热塑性塑料的情况下为1 µm–10 mm，在金属基体的情况下为300 µm–750 µm，在玻璃的情况下为750µm–3 mm，
层B：40 nm – 250 nm，
层C：80 nm – 250 nm，
层D：80 nm – 250 nm，
层E：1 nm – 200 nm。
9.根据权利要求1的多层结构，其中层A具有1mm-5mm的总层厚度。
10.根据权利要求1的多层结构，其中层B的层厚度为80-130nm。
11.根据权利要求1的多层结构，其中层B由钛组成且具有105nm-120nm的层厚度。
12.根据权利要求1的多层结构，其中层C的层厚度为90nm-160nm，层D的层厚度为90nm-160nm和层E的层厚度为20nm-100nm。
13.根据权利要求1的多层结构，其中所述热塑性塑料选自聚碳酸酯、芳族聚酯和聚碳酸酯共混物，其中这些热塑性塑料可以含有填料。
14.根据权利要求1的多层结构的用途，作为光伏模块、太阳能模块和照明系统中的反射器，作为住宅领域中和车辆领域中的反射镜和作为光导系统中的反射器。
15.光伏模块、太阳能模块、照明系统和光导系统，其包含根据权利要求1的多层结构。
16.反射镜，其包含根据权利要求1的多层结构。
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