CN1106937C - 带有附加涂层或附加层的多层聚合物薄膜 - Google Patents
带有附加涂层或附加层的多层聚合物薄膜 Download PDFInfo
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- CN1106937C CN1106937C CN96196475A CN96196475A CN1106937C CN 1106937 C CN1106937 C CN 1106937C CN 96196475 A CN96196475 A CN 96196475A CN 96196475 A CN96196475 A CN 96196475A CN 1106937 C CN1106937 C CN 1106937C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y10T428/00—Stock material or miscellaneous articles
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- Y10T428/2495—Thickness [relative or absolute]
- Y10T428/24967—Absolute thicknesses specified
- Y10T428/24975—No layer or component greater than 5 mils thick
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/28—Web or sheet containing structurally defined element or component and having an adhesive outermost layer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
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- Y10T428/31786—Of polyester [e.g., alkyd, etc.]
Abstract
本发明涉及含有光学叠层的多层聚合物薄膜,所述光学叠层包括多层交替聚合物层,表皮层具有不同于所述光学叠层中各层的机械、光学或化学性能。
Description
发明背景
众所周知,多层光学叠层可用于提供多种光学性能。这些多层叠层可用作反射偏振器或反射镜,反射所有偏振光。它们也可用作波长选择性反射体,如反射可见光而透射红外光的“冷反射镜”,或者透射可见光而反射红外光的“热反射镜”。在1995年3月10日递交的美国专利申请08/402,041中提到了多种可构成的多层叠层的实例。
现有技术中已知的多层叠层的问题在于这些叠层本身不具有所有所需的物理、化学或光学性能。因此其它能提供这些所需的性能的方法将是有用的。
发明综述
根据本发明的一个实例,在多层薄膜的一个或两个主表面上粘附至少一层附加层,该附加层具有选定的不同于光学叠层材料的机械、化学或光学性能。
根据本发明的另一个实例,在多层薄膜的一个或两个主表面上粘附至少一层附加层,该附加层将保护多层光学叠层。
附图的简要说明
图1A和1B以及图2显示了本发明较佳的多层光学薄膜;
图3至图8显示了实施例1-6中所述的多层光学薄膜的透射光谱;
图9显示了本发明的在一个主表面粘附有附加层的多层薄膜;
图10显示了本发明的在两个主表面都粘附有附加层的多层薄膜;
图11显示了在一个主表面粘附有一层附加层,而在另一个主表面粘附有两层附加层的多层薄膜。
发明详述
多层光学薄膜
多层光学薄膜的优点、特性以及这些薄膜的制造在1995年3月10日递交的尚未授权且共同转让的题为光学薄膜的美国专利申请08/402,041的申请文本中作了很详细的说明,该专利文献在此引作参考。多层光学薄膜可用作高效反射镜和/或偏振器。下面简要说明该多层光学薄膜的性能和特点,然后说明使用本发明的多层光学薄膜的反光系统的说明性实施方案。
本发明中使用的多层光学薄膜对入射光的吸收相对较低,且对于离轴及法向光线的反射性高。无论这些薄膜是用于纯反射,还是用于光的反射偏振,通常都具有这些性能。由于多层光学薄膜具有这些独特的性能和优点,因此可设计出与已知的反光系统相比,具有低的吸收损耗的高效反光系统。
如图1A和1B所示,本发明的多层光学薄膜包括多层叠合膜10,它包括至少两种材料12和14的交替叠层。其中至少有一种材料具有应力诱导双折射(stressinduced birefringence)的性能,即材料的折射率(n)受拉伸的影响。图1A显示了拉伸之前的典型的多层叠合膜,其中两种材料具有相同的折射率。光线13几乎没有感受到不同的折射率并通过该多层叠合膜。在图1B中,对同一多层叠合膜进行了拉伸,这样提高了材料12的折射率。在各层之间的界面处的折射率之差将导致光线15部分反射。通过在单轴取向至双轴取向范围拉伸该多层叠合膜,可产生对于不同取向的平面偏振入射光具有一定范围内的反射性的薄膜。因此这种多层叠合膜可用作反射偏振器和反射镜。
本发明的多层光学薄膜对于聚合物层界面的布儒斯特角(即对于在任何层界面的入射光反射率趋近零的角度)很大或不存在。与此相反,已知的多层聚合物薄膜在层界面具有相对小的布儒斯特角,导致光的透射和/或产生不希望有的晕色。而本发明的多层光学薄膜可构成其p偏振光反射率随偏离法线的入射角而缓慢地减小、与入射角无关或者随入射角而增大的多层反射镜和偏振器。结果可得到在阔的带宽下和在很宽的角度范围内对s和p偏振光都具有高反射率的多层叠合膜。
图2显示了多层叠合膜中的两层,并标明每层的三维折射率。102层的折射率为n1x、n1y和n1z,104层的折射率为n2x、n2y和n2z。两层薄膜相互之间以及与多层叠合膜中其它层之间折射率的关系决定了多层叠合膜对来自任何方位以任何角度入射的光的反射性能。在美国专利申请No.08/402,041中所述的原理和设计考虑可用于产生对于多种情况和用途具有所需的光学效应的多层叠合膜。可控制和调节多层叠合膜中各层的折射率以产生所需的光学性能。
再参见图1B,多层叠合膜10可包括几十、几百或几千层,每层可由许多种材料中的任何材料构成。根据何种特征来选择用于一特定叠合膜的材料,取决于该叠合膜所需的光学性能。叠合膜所含材料的种类可与其层数相同。但为了便于制造,较佳的光学叠合薄膜只含有数目不多的不同材料。
材料之间的分界面,或者化学上相同而物理性质不同的材料之间的分界面,可以是突变的或是渐变的。除了某些具有分析解的简单情况以外,对后一种类型折射率连续变化的分层介质的分析,通常都作为具有非常多均匀薄层,各层间的界面是突变的,但相邻的层之间性质变化很小的情况来处理。
理想的多层叠合薄膜含有许多高/低折射率薄膜层组,每组高/低折射率层的总光学厚度是设计的反射频带中心波长的1/2。这类薄膜的叠合膜一般称为1/4波长叠合膜。对于与可见和近红外波长有关的多层光学薄膜,设计四分之一波长叠层将使多层叠层中的每一层的平均厚度不大于0.5微米。
在需要反射薄膜的应用中(如反射镜),所希望得到的对每种偏振和每种入射平面的光的平均透射率,一般取决于反射薄膜的计划用途。生成多层反射镜薄膜的一种方法是双轴向拉伸多层叠层。高效反射薄膜在法向入射时沿每一拉伸方向在可见光谱范围(380-750nm)的平均透射率要求在10%以下(反射率大于90%),较好是5%以下(反射率大于95%),更好是2%以下(反射率大于98%),最好是1%以下(反射率大于99%)。在偏离法向60°可见光谱范围(380-750nm)的平均透射率要求在20%以下(反射率大于80%),较好是10%以下(反射率大于90%),更好是5%以下(反射率大于95%),还要好是2%以下(反射率大于98%),最好是1%以下(反射率大于99%)。
此外,在某些应用中可能需要不对称的反射薄膜。例如,在可见光谱范围(380-750nm)或在可见至近红外范围(380-850nm),沿一个拉伸方向的平均透射率小于50%,而沿另一个拉伸方向的平均透射率则小于20%。
多层光学薄膜也可设计成反射偏振器。生成多层反射偏振器的一种方法是单轴向拉伸多层叠层。得到的反射偏振器在广阔的入射角范围内对偏振面平行于一个轴的光(在拉伸方向)具有高反射率,而同时对偏振面平行于另一个轴的光(在非拉伸方向)具有低反射率和高透射率。控制每层薄膜的三个折射率nx、ny和nz,可以得到所需的偏振器性能。
对于许多应用,理想的反射偏振器在所有的入射角下沿一个轴上(所谓消光轴)具有高反射率而沿另一个轴上(所谓透射轴)的反射率为零。对于偏振器的透射轴,一般要求沿透射轴方向偏振的光在所考虑的带宽范围内以及在所考虑的角度范围内的透射率达到极大。
偏振器在可见光谱范围(380-750nm,带宽300nm)法向入射的光在透射轴上的平均透射率一般要求至少为50%,较好为至少70%,更好为至少85%,最好为至少90%。偏振器在380-750nm范围对偏离法线60°的入射光的平均透射率(沿透射轴测量)一般要求至少为50%,较好为至少70%,更好为至少80%,最好为至少90%。
多层反射偏振器对可见光谱范围(380-750nm,带宽300nm)法向入射在消光轴方向偏振的光的平均透射率一般要求小于50%,较好为小于30%,更好为小于15%,最好为小于5%。偏振器对在消光轴方向偏振的光在380-750nm范围偏离法线60°入射时的平均透射率(沿p-偏振光的透射轴测量)一般要求小于50%,较好为小于30%,更好为小于15%,最好为小于5%。
在某些应用中,要求在偏离法向的角度下对于偏振平面与透射轴平行的p-偏振光具有高反射率。对于沿透射轴偏振的光在偏离法线的角度至少为20°时的平均透射率应大于20%。
另外,虽然在此对反射偏振薄膜和不对称反射薄膜分别进行了讨论,但应该理解可将两种或多种这样的薄膜装置成基本上反射所有入射在其上的光线(条件是它们相互之间适当地取向)。当根据本发明多层光学薄膜用作反光系统中的反射器时通常需要这样的结构。
如果沿透射轴发生一定的反射,偏振器在偏离法线的角度下的效率就会降低。如果沿透射轴的反射率对各种波长是不同的,透射光中就会引入颜色。测定颜色的一种方法,是确定在某一选定角度下或某几个选定角度下,在所考虑的波长范围内的透射率的方均根值(RMS)。%方均根色彩CRMS可由以下公式确定:
其中λ1至λ2是考虑的波长范围或带宽,T是沿透射轴的透射率,
T是在考虑的波长范围内沿透射轴的平均透射率。对于要求一个低色度偏振器的应用,在偏离法线的角度至少为30°(较好至少为45°,最好至少为60°)时,其%RMS色彩应低于10%(较好为低于8%,更好为低于3.5%,最好为低于2%)。
较好的是,反射偏振器将特别应用中所需的沿透射轴的%RMS色彩与在考虑的带宽范围内所需的沿消光轴的反射率结合起来。对于带宽在可见光谱范围(400-700nm,或带宽为300nm)的偏振器,法向入射时沿消光轴的平均透射率一般要求小于40%,较好为小于25%,更好为小于15%,最好为小于5%,尤其好是小于3%。
材料选择与处理
根据上面提到的美国专利申请No.08/402,041中所述的设计考虑,本领域普通技术人员会容易地理解,当在选定的条件下进行处理以产生所需折射率关系,有非常多材料可用来构成本发明的多层反射薄膜或偏振器。所需的折射率关系可用各种方法得到,包括在薄膜形成过程中或形成以后拉伸(例如在有机聚合物的情况),挤塑(例如在液态结晶材料的情况),或涂敷。此外,最好两种材料具有相似的流变性质(如熔体粘度),以便可进行共挤塑。
一般可选择结晶或半结晶或者液晶材料(较好是聚合物)作为第一种材料以获得适当的组合。第二种材料本身可以是结晶的、半结晶的或非晶形的。第二种材料可以具有与第一种材料相反或相同的双折射。或者第二种材料可以不具有双折射。应该理解在聚合物技术领域,通常认为聚合物一般不是完全结晶的,因此在本发明中,结晶或半结晶聚合物是指不是无定形的聚合物,包括任何通常称作结晶、部分结晶、半结晶等的材料。
适合的材料的具体例子包括聚萘二甲酸乙二醇酯(PEN)及其异构体(如2,6-、1,4-、1,5-、2,7-和2,3-PEN);聚对苯二甲酸烷二醇酯(如聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯、和聚-1,4-环己烷二亚甲基对苯二甲酸酯);聚酰亚胺(如聚丙烯酰亚胺);聚醚酰亚胺(polyetherimide);无规立构的聚苯乙烯;聚碳酸酯;聚甲基丙烯酸酯(如聚甲基丙烯酸异丁酯、聚甲基丙烯酸丙酯、聚甲基丙烯酸乙酯、和聚甲基丙烯酸甲酯);聚丙烯酸酯(如聚丙烯酸甲酯和聚丙烯酸丁酯);间同立构的聚苯乙烯(sPS);间同立构的聚-α-甲基苯乙烯;间同立构的聚二氯苯乙烯;任何这些聚苯乙烯的共聚物和掺合物;纤维素衍生物(如乙基纤维素、乙酸纤维素、丙酸纤维素、乙酸-丁酸纤维素、和硝酸纤维素);聚烯烃聚合物(如聚乙烯、聚丙烯、聚丁烯、聚异丁烯、和聚(4-甲基)戊烯);氟化的聚合物(如全氟烷氧基树脂、聚四氟乙烯、氟化的乙烯-丙烯共聚物、聚偏二氟乙烯、和聚氯三氟乙烯);氯化的聚合物(聚偏二氯乙烯、和聚氯乙烯);聚砜;聚醚砜;聚丙烯腈;聚酰胺;硅氧烷树脂;环氧树脂;聚乙酸乙烯酯;聚醚-酰胺;离子键树脂;弹性体(如聚丁二烯、聚异戊二烯、和氯丁橡胶);和聚氨酯。也可使用共聚物,例如PEN的共聚物[如2,6-、1,4-、1,5-、2,7-、和/或2,3-萘二甲酸或其酯与以下物质的共聚物:(a)对苯二甲酸或其酯;(b)间苯二甲酸或其酯;(c)邻苯二甲酸或其酯;(d)烷烃二醇;(e)环烷烃二醇(例如环己烷二甲醇);(f)烷烃二羧酸;和/或(g)环烷烃二羧酸(例如环己烷二甲酸)],聚对苯二甲酸烷二醇酯的共聚物[如对苯二甲酸或其酯与以下物质的共聚物:(a)萘二甲酸或其酯;(b)间苯二甲酸或其酯;(c)邻苯二甲酸或其酯;(d)烷烃二醇;(e)环烷烃二醇(例如环己烷二甲醇);(f)烷烃二羧酸;和/或(g)环烷烃二羧酸(例如环己烷二甲酸)],苯乙烯共聚物(例如苯乙烯-丁二烯共聚物和苯乙烯-丙烯腈共聚物),以及4,4’-二苯甲酸与1,2-乙二醇的共聚物。此外,每一单独的层可包括两种或多种上述聚合物或共聚物的掺合物(如sPS与无规立构聚苯乙烯的掺合物)。所述的coPEN也可以是颗粒的掺合物,其中至少一个组分是以萘二甲酸为基的聚合物,而其它的组分是其它聚酯或聚碳酸酯,如PET、PEN或co-PEN。
在偏振器的情况,特别好的层的组合包括PEN/coPEN,聚对苯二甲酸乙二醇酯(PET)/coPEN,PEN/sPS,PET/sPS,PEN/Estar,和PET/Estar,其中“co-PEN”是(如上所述的)以萘二甲酸为基的共聚物或掺合物,而Estar是可购自Eastman Chemical Co的聚环己烷二亚甲基对苯二甲酸酯。
在反射薄膜的情况,特别好的层的组合包括PET/Ecdel,PEN/Ecdel,PEN/sPS,PEN/THV,PEN/co-PET,和PEN/sPS,其中“co-PET”是(如上所述的)以对苯二甲酸为基的共聚物或掺合物,Ecdel是可从Eastman Chemical Co购得的热塑性聚酯材料,而THV是可从美国明尼苏达州的美国3M公司购得的含氟聚合物。
薄膜的层数,考虑到膜的厚度、柔软性和经济原因,是选择得用最少的层数达到所需的光学性能。在偏振器和反射薄膜的情况,层数都较好在10,000以下,更好在5,000以下,最好在2,000以下。
如上所述,获得各折射率之间所需关系(因而获得多层膜的光学性能)的能力,受到制备该多层膜所用处理条件的影响。在可通过拉伸而取向的有机聚合物的情况,通常是将各聚合物共挤塑形成多层膜,然后在选定温度下拉伸使其取向,再(可任选地)在预定的温度下热固化,以制得该薄膜。另外一种方法,是同时进行挤塑和取向步骤。在偏振器的情况,薄膜在一个方向上被显著地拉伸(单轴取向),而在反射薄膜的情况。薄膜在两个方向上被显著地拉伸(双轴取向)。
可以让薄膜在拉伸的横向上,从自然的拉伸横向收缩(等于拉伸比的平方根)发生尺寸松弛,可简单地使拉伸横向的尺寸无任何明显变化,或者可以在拉伸横向主动拉伸。薄膜可以在机器方向拉伸(用长度取向器)或用拉幅机沿宽度方向拉伸。
拉伸前温度、拉伸温度、拉伸速率、拉伸比、热固化温度、热固化时间、热固化松弛以及拉伸横向松弛等条件是选择得可产生具有所需折射率关系的多层膜。这些变量是互相依赖的;于是,如果与较低的拉伸温度相结合,可使用较低的拉伸速率。本领域普通技术人员会容易地选取这些变量的适当组合,以得到所需的多层薄膜。但是,一般较佳的拉伸比在拉伸方向为1∶2至1∶10(更好为1∶3至1∶7)而在与拉伸方向垂直的方向为1∶0.2至1∶10(更好为1∶0.2-1∶7)。
也可以采用以下技术来制备合适的多层膜:旋转涂覆(参看Boese等,J.Polym.Sci.;Part B,30:1321(1992))用以制备双折射聚酰亚胺膜,以及真空沉积(参看Zang等人,Appl.Phys.Letters,59:823(1991))用以制备结晶有机化合物膜;后一种技术对某些结晶的有机化合物和无机材料的组合特别适用。
以下通过实施例来说明多层反射镜薄膜和多层反射偏振器。
实施例1(PEN:THV,500,449,反射镜)
在一次操作中挤塑流延的片料,然后在实验室用薄膜拉伸器中使薄膜取向,制得包含449层的共挤塑膜。用一台挤塑机以56lb/hr的速率输送特性粘度为0.53dl/g(60重量%苯酚/40重量%二氯苯)的聚萘二甲酸乙二醇酯(PEN),而用另一台挤塑机以11lb/hr的速率输送THV 500(购自美国3M公司的含氟聚合物)。PEN在表皮层中,50%的PEN存在于两层表皮层中。用供料头方法产生57层,再将其通过三个倍增器,得到449层的挤塑制品。流延片料是20密耳厚,12英寸宽。然后用实验室薄膜拉伸装置使片料双轴取向,该装置用一个缩放架夹住一个方块的薄膜,并以均匀的速率同时在两个方向拉伸它。将7.46厘米平方的片料在约100℃下装入拉伸器,在60秒内加热至140℃。然后以每秒10%的速率(基于原来的尺寸)开始拉伸,直至将样品拉伸至3.5×3.5。紧接在拉伸后,用室温的空气吹在样品上面使其冷却。
图3显示了该多层膜的透射率。曲线(a)显示了在透射方向的偏振光法向入射时的响应,而曲线(b)显示了在透射方向偏振的p-偏振光60°时的响应。
实施例2(PEN:PMMA,601,反射镜)
在连续展平-制膜生产线上通过共挤塑过程制得包含601层的共挤塑薄膜。用挤塑机A以114lb/hr的速率输送特性粘度为0.57dl/g(60重量%苯酚/40重量%二氯苯)的聚萘二甲酸乙二醇酯(PEN),其中64lb/hr进入供料头(feedblock),其余的进入下述的表皮层。用挤塑机B以61lb/hr的速率输送PMMA(购自ICI ofAmericas的CP-82),均进入供料头。PEN是在供料头的表皮层。用供料头方法(使用美国专利3,801,429中所述的供料头)产生151层,然后用挤塑机C以30lb/hr的数量输送挤塑机A所输送的相同类型的PEN,共挤塑两层对称的表皮层。使该挤出物通过两个倍增器,得到601层的挤塑制品。美国专利3,565,985说明了类似的共挤塑倍增器。挤出物通过另一装置,使来自挤塑机A的PEN以50lb/hr的总速率共挤塑表皮层。片料在片温约280°F下进行长度取向至拉伸比约为3.2。随后将薄膜在约38秒内预热至约310°F,以约每秒11%的速率在横向拉伸至拉伸比约为4.5。然后让薄膜在440°F热固化而不让它松弛。最终的薄膜厚度约为3密耳。
如图4中的曲线(a)所示,法向入射的带宽约为350nm,平均带内消光率(in-band extinction)大于99%。由于光吸收值很小,难以测定,但该值小于1%。当入射角偏离法向50°时,s-偏振光(曲线(b))和p-偏振光(曲线(c))显示出类似的消光率,消光带如预期的向较短波长方向偏移。s-偏振光消光带的红色边缘向蓝色方向的偏移没有p-偏振光那么多,这是由于s-偏振光预期的较大的带宽,以及由PEN层中的p-偏振光所见的较低的折射率所致。
实施例3(PEN:PCTG,449,偏振器)
在一次操作中挤塑流延片料,然后在实验室薄膜拉伸装置中使薄膜取向,制得包含481层的共挤塑膜。用供料头方法使用61层供料头和三个(2×)倍增器。在最后一个倍增器和模头之间加入厚的表皮层。用一台挤塑机以25.0lb/hr的速率输送特性粘度为0.47dl/g(60重量%苯酚/40重量%二氯苯)的聚萘二甲酸乙二醇酯(PEN)至供料头。用另一台挤塑机以25.0lb/hr的速率输送二元醇改性的聚对苯二甲酸亚乙基二甲基环己酯(polyethylene dimethyl cyclohexane terephthalate)(购自Eastman的PCTG 5445)。将来自上述挤塑机的另一PEN流以25.0lb/hr的速率在倍增器之后作为表皮层。流延片料的厚度为0.007英寸,宽度为12英寸。然后用实验室拉伸装置使片料单轴取向,该装置用一个缩放架夹住一块薄膜,以均匀速率沿一个方向拉伸,而在另一个方向自由松弛。该片料样品的宽度为5.40cm(松弛方向),缩放架夹子之间长为7.45cm。在约100℃下将片料装入拉伸器,并在135℃加热45秒。然后以每秒20%的速率开始拉伸(基于原来的尺寸),直至样品被拉伸至约6∶1(基于夹子至夹子的测定值)。紧接在拉伸之后,用室温空气吹向样品使其冷却。在中部,样品的松弛系数为2.0。
图5显示了该多层膜的透射率,其中的曲线a显示了在非拉伸方向偏振的光法向入射时的透射率,曲线b显示了在非拉伸方向偏振的p-偏振光在60°入射时的透射率,曲线c是在拉伸方向偏振的光法向入射时的透射率。对于曲线a,在400-700nm的平均透射率为89.7%,对于曲线b,在400-700nm的平均透射率为96.9%,对于曲线c,在400-700nm的平均透射率为4.0%。曲线a的%RMS色彩是1.05%,曲线b的%RMS色彩是1.44%。
实施例4(PEN:coPEN,601,偏振器)
通过共挤塑方法在连续展平-制膜生产线上制得包含601层的共挤塑膜。用一台挤塑机以75lb/hr的速率输送特性粘度为0.54dl/g(60重量%苯酚/40重量%二氯苯)的聚萘二甲酸乙二醇酯(PEN),而用另一台挤塑机以65lb/hr的速率输送coPEN。coPEN为70摩尔%2,6-萘二甲酸甲酯、15摩尔%间苯二甲酸二甲酯和15摩尔%对苯二甲酸二甲酯与乙二醇的共聚物。用供料头方法产生151层膜。供料头设计成能产生从顶部到底部具有厚度梯度分布,从最薄层到最厚层的厚度比例为1.22的薄膜叠层。将PEN表皮层共挤塑在光学叠合膜的外侧,总厚度为共挤塑层的8%。光学叠合膜用两个串连的倍增器使其层数倍增。倍增器的标称倍增比分别为1.2与1.27。然后在约40秒内将薄膜预热至310°F,并以约每秒6%的速率在横向拉伸,直至拉伸率约为5.0。最终的薄膜厚度约为2密耳。
该多层膜的透射率如图6如示。曲线a显示了在非拉伸方向偏振的光法向入射时的透射率,曲线b显示了p-偏振光60°入射时的透射率,曲线c显示了在拉伸方向偏振的光法向入射时的透射率。注意在非拉伸方向的p-偏振光法向入射时和60°入射时的透射率都非常高(80%-100%)。如曲线c所示,在可见光范围内(400-700nm)在拉伸方向偏振的光的消光率非常高。在500至650nm消光率接近100%。
实施例5(PEN:sPS,481,偏振器)
用购自Eastman Chemicals的特性粘度为0.56dl/g(在60重量%苯酚和40重量%二氯苯中测得)的聚萘二甲酸乙二醇酯(PEN)和间同立构的聚苯乙烯(sPS)均聚物(重均分子量=200,000道尔顿,由Dow Corporation供样)制得包含481层的多层膜。PEN是在外部的层中,是以26lb/hr的速率挤塑,而sPS是以23lb/hr的速率挤塑。所用的供料头产生61层,每层的厚度近似相等。在供料头后面,使用了三个(2x)倍增器。在最后的倍增器以后,以22lb/hr的总速率加入相同厚度的表皮层(它们含有与输入至供料头相同的PEN)。片料是通过12”宽的模头,挤塑至厚度约为0.011英寸(0.276mm)。挤塑温度为290℃。
将这片料在环境条件下储放9天,然后在拉幅机上使其单轴取向。在约25秒内将膜预热至约320°F(160℃),并以每秒约28%的速率在横向拉伸至拉伸比约为6∶1。没有让片料在拉伸方向松弛。最终薄膜厚度约为0.0018英寸(0.046mm)。
图7显示了包含481层的这一PEN:sPS反射偏振器的光学性能。曲线a显示了在非拉伸方向偏振的光法向入射时的透射率,曲线b显示了p偏振光在60°入射时的透射率,曲线c是在拉伸方向偏振的光法向入射时的透射率,注意p偏振光法向入射时和60°入射时都具有很高的透射率。曲线a在400-700nm范围的平均透射率是86.2%,而曲线b在400-700nm范围的平均透射率是79.7%。曲线c上可看到在拉伸方向偏振的光在可见光谱范围(400-700nm)具有很高的反射率。曲线c上膜在400-700nm范围内的平均透射率为1.6%。曲线a的%RMS色彩是3.2%,曲线b的%RMS色彩是18.2%。
实施例6(PEN:coPEN,603,偏振器)
在连续展平-制膜生产线上通过共挤塑过程制得包含603层的反射偏振器。用一台挤塑机以83lb(38kg)/hr的速率输送特性粘度为0.47dl/g(在60重量%苯酚/40重量%二氯苯中)的聚萘二甲酸乙二醇酯(PEN),而用另一台挤塑机以75lb(34kg)/hr的速率输送coPEN。所用的coPEN是70摩尔%2,6-萘二甲酸甲酯,15摩尔%对苯二甲酸二甲酯和15摩尔%间苯二甲酸二甲酯与1,2-乙二醇的共聚物。用供料头方法产生151层。供料头设计成可使光学叠合膜从底部到顶部的层厚产生一梯度,从最薄层到最厚层的厚度比为1.22。光学叠合膜用两个串连的倍增器使其层数倍增。倍增器的标称倍增比分别为1.2与1.4。在最后的倍增器和模头之间加入由上述同样的coPEN制成的由第三台挤塑机以106lb(48kg)/hr的总速率输送的表皮层。然后在约30秒内将膜预热至300°F(150℃),以每秒20%的初始速率在横向拉伸至拉伸比约为6。最终薄膜的厚度为约0.0035英寸(0.089mm)。
图8显示了实施例6的偏振器的光学性能。曲线a显示了在非拉伸方向偏振的光法向入射时的透射率,曲线b显示了在非拉伸方向的p偏振光50°(偏离法向)入射时的透射率,曲线c是在拉伸方向偏振的光法向入射时的透射率。注意在非拉伸方向偏振的光具有很高的透射率。曲线a在400-700nm范围的平均透射率是87%。曲线b上可看到在拉伸方向偏振的光在可见光谱范围(400-700nm)具有很高的反射率。曲线b上膜在400-700nm范围内的平均透射率为2.5%。而且,该偏振器的%RMS色彩很低。曲线b的%RMS色彩是5%。
虽然如上所述的多层光学叠层可提供重要的和所需的光学性能,但难以在光学叠层本身中提供其它性能(如机械、光学或化学性能)而不破坏该光学叠层的性能。这些性能可通过在光学叠层中包含一层或多层薄层而提供,这些薄层能提供这些性能而不影响光学叠层本身原有的光学性能。由于这些薄层通常位于光学叠层的主表面上,因此它们常被称作“表皮层”。
表皮层可在制备多层叠层时共挤塑在其一个或两个主表面上以保护多层叠层不受沿供料头和模头壁的高剪切力,通过将诸如紫外光稳定剂等添加剂混入形成表皮层的聚合物熔料中,在制备时将该具有改变的性能的表皮层共挤塑至多层光学叠层的一面或两面,常常能得到具有所需的化学或物理性能的外层。该附加层也可以在制备多层薄膜时共挤塑在表皮层的外面;它们可以用单独的涂覆操作涂覆在多层薄膜上;或者可以作为独立的膜、箔或者刚性或半刚性增强基材(如聚酯(PET)、丙烯酸类(PMMA)、聚碳酸酯、金属或玻璃)与多层薄膜层压在一起。可用于将多层聚合物薄膜与另一表面层压在一起的添加剂包括光学透明的和漫射的粘合剂,以及包括压敏的和非压敏的粘合剂。压敏粘合剂通常在室温下是发粘的,最多用手指轻压就可使其粘附于表面,非压敏粘合剂包括溶剂、热或辐射活化的粘合剂体系。本发明中有用的粘合剂的实例包括基于聚丙烯酸酯的一般组合物的那些粘合剂;聚乙烯基醚;含二烯的橡胶(如天然橡胶、聚异戊二烯和聚异丁烯);聚氯丁二烯;丁基橡胶;丁二烯-丙烯腈聚合物;热塑性弹性体;嵌段共聚物(如苯乙烯-异戊二烯和苯乙烯-异戊二烯-苯乙烯嵌段共聚物,乙烯-丙烯-二烯聚合物,以及苯乙烯-丁二烯聚合物);聚-α-烯烃;非晶型聚烯烃;聚硅氧烷;含乙烯的共聚物(如乙烯乙酸乙烯酯,丙烯酸乙酯和甲基丙烯酸乙酯);聚氨酯;聚酰胺;环氧树脂;聚乙烯吡咯烷酮和乙烯吡咯烷酮共聚物;聚酯;以及它们的混合物。另外,这些粘合剂可含有诸如增粘剂、增塑剂、填料、抗氧化剂、稳定剂、颜料、散射颗粒、固化剂、生物杀伤剂和溶剂等添加剂。可用于本发明的较好的粘合剂包括Shell Chemical Co.(Akron,OH)有售的热熔粘合剂VITEL 3300,或者丙烯酸压敏粘合剂,如明尼苏达州的美国3M公司有售的90/10 IOA/AA丙烯酸粘合剂。当层压粘合剂用于将多层薄膜粘附于另一表面时,最好选择粘合剂组成和厚度使多层叠层的光学性能不受影响。例如,当将附加层与要求具有高透射率的多层聚合物偏振器或反光镜层压在一起时,在偏振器或反射镜设计成透明的波长范围内,该层压粘合剂应是光学透明的。
图10和11说明分别具有一层和两层附加层的多层叠层。下面用图10和11说明各种可施用的附加层。
其中的表皮层最好具有不同的机械性能的一个领域尤其涉及单轴取向的多层光学叠层,如反射偏振器。这些叠层常显示出在主要拉伸方向抗撕裂性低。这会导致在制造过程中产率降低,或者导致薄膜在随后的处理时断裂。为了防止出现这些现象,可将耐撕裂层粘附于光学叠层的外主表面。这些坚韧的层可以是任何适宜的材料,甚至可以与光学叠层中所用的材料中的一种相同。在选择耐撕裂层材料时考虑的因素包括断裂伸长百分数、杨氏模量、撕裂强度、对内层的粘附性、在所考虑的电磁带宽的透射率和吸收率、光学透明度或雾度、作为频率函数的折射率、质地和粗糙度、熔体热稳定性、分子量分布、熔融流变性和共挤塑性、坚韧层和光学层中材料之间的混溶性和相互扩散速率、粘弹响应、在拉伸条件下的松弛和结晶性能、在使用温度下的热稳定性、耐天候性、粘附于涂层的能力以及对各种气体和溶剂的渗透性。当然,如上所述,重要的是所选的材料不具有对光学叠层不利的光学性能。它们可在制备过程中施用,或者随后涂覆于光学叠层上或与光学叠层层压在一起。在制备过程(如共挤塑过程)中将这些薄层粘附于光学叠层的优点在于在制备过程中光学叠层受到保护。
用图10说明本发明的这一方面,图中可见带有耐撕裂层的多层光学叠层400。薄膜400含有光学叠层410。光学叠层410含有两种具有不同光学性能的聚合物的交替层412和414。在光学叠层410的主表面粘附有耐撕裂层416和418。应该注意,虽然从图10中看416和418层比412和414层厚,但图10并不代表通常优选的实施方案。一般来说较好的是各416和418层的厚度大于光学叠层厚度的5%。较好的是各416和418层的厚度为光学叠层厚度的5%至60%,以提供抗撕裂性而不必增加所用材料的量。因此,如果光学叠层具有600层,在该优选的实施方案中,各耐撕裂层416和418的厚度等于30至360层的叠层的厚度。在更优选的实施方案中,各耐撕裂层416和418的厚度为光学叠层厚度的30%至50%。
在特别理想的实施方案中,耐撕裂外层可以是与交替层412和414所用材料中的一种相同的材料。尤其是现已发现在含有PEN和coPEN交替层的反射偏振器中,coPEN耐撕裂外层可在制备过程中共挤塑。
实施例7
将由多层交替层PEN和coPEN的复合物形成的反射偏振器与coPEN的厚表皮层共挤塑,形成耐撕裂反射偏振器。在连续展平-薄膜挤塑机上制成含603层的共挤塑薄膜。用一台挤塑机以86lb/hr的速率输送特性粘度为0.47dl/g(60重量%苯酚/40重量%二氯苯)的聚萘二甲酸乙二醇酯(PEN),而用另一台挤塑机以78lb/hr的速率输送coPEN。coPEN为70摩尔%2,6-萘二羧酸甲酯和30摩尔%对苯二甲酸二甲酯与乙二醇的共聚物。用供料头挤塑出151层膜。供料头设计成能产生从顶部到底部具有厚度梯度分布,从最薄层到最厚层的厚度比例为1.22的薄膜叠层。该光学叠合膜用两个串连的倍增器使其层数倍增。倍增器的标称倍增比分别为1.2与1.27。在最后的倍增器和模具之间加入上述含有coPEN的薄层。这些薄层通过第三台挤塑机以187lb/hr的最终速率加入和输送。在约40秒内将带有附加的coPEN外层的薄膜预热至320°F,并以约每秒20%的初始速率在横向拉伸,直至拉伸率约为6。最终的薄膜厚度约为100微米,包括约50微米厚的内部多层光学叠层和厚度各为约25微米的两层外层(在薄膜的每一面上)。比没有表皮层的情况提高了抗撕裂性,就可生产成卷的缠绕坚韧反射偏振器。具体来说,根据ASTM D-1938,用裤型撕裂试验沿主要拉伸方向测定根据本实施例制备的薄膜以及在相同条件下制备但没有coPEN表皮层的薄膜的抗撕裂性。薄膜的平均厚度分别为100微米和48微米。平均撕力值为60.2和2.9克力,标准偏差分别为4.44和0.57克力。对coPEN表皮层的分析显示出低的向,在633nm处折射率为1.63、1.62和1.61。难以使该结构干净地分离表明具有良好的层间粘合性。为了进一步进行比较,对具有3.8微米PEN外层的48微米光学叠层进行了测定,发现平均撕力为2.8克,标准偏差为1.07。
薄膜的外观和/或性能可通过包含带有吸收光谱中一个或多个选定范围的染料或颜料的表皮层而改变。这可包括部分或全部可见光谱以及紫外和红外光谱。当然,如果吸收全部可见光谱,则该层将是不透明的。可进行选择以改变通过薄膜透射或反射的光线的表观颜色。它们也可用于提高薄膜的性能,尤其是透射某些频率而反射其它频率的薄膜。在外层使用紫外吸收材料是特别理想的,因为它可用于保护当受到紫外辐射时会不稳定的内层。图9说明了表示带有含电磁吸收材料的316层的薄膜。
与上述电磁吸收材料相类似,可将荧光材料加入图9中的316层中或者图9中的416和418中的一层或两层中。荧光材料吸收光谱中紫外光范围的电磁能量而重发射可见光。理想的荧光材料包括受阻胺光稳定剂(HALS),在1994年11月28日递交的美国专利申请08/345,608中对此有更详细的叙述,该专利文献在此引作参考。
压敏粘合剂是另一类可作为图9中的316层或图10中的416层或418层用于多层叠层的理想的材料。一般来说,压敏粘合剂可在需将光学叠层与另一种材料(如玻璃或金属基材)进行层压时施用。
可加入表皮层(如316层或416层或418层)的另一种材料为滑爽剂。滑爽剂使薄膜在制备过程中更易处理。通常滑爽剂与反射镜薄膜(而不是需透射部分光线的薄膜)一起使用。包含滑爽剂的一面通常需与支撑基材进行层压,以防止因滑爽剂反射而导致雾度增加。
另一类可采用的附加层为保护层。该层可以是耐磨的或者耐老化和/或耐化学作用的。当多层薄膜会暴露于苛刻的或腐蚀性环境时这些涂层是特别有用的。耐磨的或坚硬的涂层实例包括丙烯酸硬涂层(hardcoat),如购自Rohm & Haas的Acryloid A-11和Paraloid K-120N;聚氨酯丙烯酸酯(urethane acrylates),如美国专利No.4,249,011中所述的和购自Sartomer Corp.的那些;以及聚氨酯硬涂层,如由脂族聚异氰酸酯(如购自Miles,Inc.的Desmodur N-3300)与聚酯(购自UnionCarbide的Tone Polyol 0305)反应得到的那些。这些涂层也可防止气体(如氧气或二氧化碳或水蒸汽)透过薄膜。同样这也可以是图9中的单一层或图10中的两表面层。
可加入的其它层包括含有全息图象、全息散射体(holographic diffusers)或其它散射层的薄层。这些薄层可在硬性聚合物中或在粘合剂中。
图11显示了带有交替层512和514与保护层516、518和520的交替多层薄膜500。多层附加层可与多层光学叠层的一个主表面相邻。使用图11中所示的结构类型的实例为如上所述保护层516和518是耐撕结构,而520层为耐磨层。
以上所述是各种可施用于多层叠层的外部以改变其性能的涂层的实例。一般来说,可加入任何具有与叠层本身不同的机械、化学或光学性能的附加层。
Claims (27)
1.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,各层在所述层平面内的折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的所述折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层的材料具有选定的机械性能,所述机械性能不同于所述光学叠层的所述各层的机械性能。
2.如权利要求1所述的多层薄膜,其特征在于还包含粘附在第二主表面上的第二附加层。
3.包含第一种和第二种聚合物层的多层光学薄膜,所述第一种和第二种聚合物的组成不同,每一层的厚度不大于0.5微米,所述第一聚合物层的层平面内折射率为n1x和n1y,与所述第一聚合物层平面正交方向的折射率为n1z,所述第二聚合物层的层平面内折射率为n2x和n2y,与所述第二聚合物层平面正交方向的折射率为n2z,选择所有所述折射率以形成所需的光学性能,所述光学叠层具有第一和第二主表面,所述第一主表面粘附有第一耐撕层。
4.如权利要求3所述的多层光学薄膜,其特征在于所述第二主表面粘附有第二耐撕层。
5.如权利要求4所述的多层光学薄膜,其特征在于每一耐撕层的厚度大于所述光学叠层厚度的5%。
6.如权利要求5所述的多层光学薄膜,其特征在于每一耐撕层的厚度为所述光学叠层厚度的5%至60%。
7.如权利要求6所述的多层光学薄膜,其特征在于每一耐撕层的厚度为所述光学叠层厚度的30%至50%。
8.如权利要求5所述的多层光学薄膜,其特征在于所述耐撕层的组成与所述第二种聚合物的组成基本相同。
9.如权利要求8所述的多层光学薄膜,其特征在于所述第一种聚合物为聚萘二甲酸乙二醇酯,所述第二种聚合物为含有萘二甲酸酯单元和对苯二甲酸酯单元的共聚多酯。
10.如权利要求3所述的多层光学薄膜,其特征在于所述第一种聚合物具有正的应力系数。
11.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,所述各层的层平面内折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层的材料具有选定的化学性能,所述化学性能不同于所述光学叠层的所述各层的化学性能。
12.如权利要求11所述的多层薄膜,其特征在于还包含粘附的第二附加层。
13.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,所述各层的层平面内折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层的材料具有选定的光学性能,所述光学性能不同于所述光学叠层的所述各层的光学性能。
14.如权利要求13所述的多层薄膜,其特征在于还包含粘附的第二附加层。
15.如权利要求1所述的多层薄膜,它还包括粘附在所述第一附加层上的第二附加层,所述第二附加层具有与所述光学叠层的各层和所述第一附加层不同的机械性能。
16.如权利要求15所述的多层薄膜,其特征在于所述第一附加层是耐撕层,所述第二附加层是耐磨层。
17.如权利要求1所述的多层薄膜,其特征在于所述第二附加层是耐磨层。
18.如权利要求1所述的多层薄膜,其特征在于所述第一附加层含有滑爽剂。
19.如权利要求13所述的多层薄膜,其特征在于所述第一附加层包括电磁吸收材料。
20.如权利要求19所述的多层薄膜,其特征在于所述电磁吸收材料吸收紫外辐射。
21.如权利要求13所述的多层薄膜,其特征在于所述第一附加层包括荧光材料。
22.如权利要求13所述的多层薄膜,其特征在于所述第一附加层包括全息图像。
23.如权利要求13所述的多层薄膜,其特征在于所述第一附加层包括全息散射体。
24.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,所述各层的层平面内折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层为压敏粘合剂层。
25.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,所述各层的层平面内折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层的材料具有选定的机械性能,所述机械性能不同于所述光学叠层的所述各层的机械性能,所述附加层是耐撕层,厚度占所述光学叠层厚度的5-60%,其组成与所述第二种聚合物的组成基本相同。
26.如权利要求25所述的多层光学薄膜,其特征在于所述第一种聚合物是聚萘二甲酸乙二醇酯,所述第二种聚合物是含萘二甲酸酯单元和对苯二甲酸酯单元的共聚聚酯。
27.含有光学叠层的多层薄膜,它包括平均厚度不大于0.5微米的半结晶聚合物层和平均厚度不大于0.5微米的第二种聚合物层,其中对所述光学叠层在至少一个方向进行拉伸至该方向未拉伸尺寸的至少两倍,所述光学叠层具有第一主表面和第二主表面,所述各层的层平面内折射率为nx和ny,与所述层平面正交方向的折射率为nz,选择所有的折射率以形成所需的光学性能,所述薄膜还包含粘附于所述第一主表面的第一附加层,所述附加层的材料具有选定的机械性能,所述机械性能不同于所述光学叠层的所述各层的机械性能,其中所述附加层是玻璃。
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- 1996-06-20 IL IL12224496A patent/IL122244A0/xx unknown
- 1996-06-20 EP EP04028333A patent/EP1537992A3/en not_active Withdrawn
- 1996-06-20 WO PCT/US1996/010691 patent/WO1997001440A1/en not_active Application Discontinuation
- 1996-06-20 AU AU63903/96A patent/AU6390396A/en not_active Abandoned
- 1996-06-20 KR KR1019970709696A patent/KR100468560B1/ko not_active IP Right Cessation
- 1996-06-20 EP EP96923376A patent/EP0836554A1/en not_active Ceased
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1997
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2008
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Cited By (4)
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CN102666093A (zh) * | 2009-12-22 | 2012-09-12 | Skc株式会社 | 双波长反射多层膜 |
CN102666093B (zh) * | 2009-12-22 | 2014-09-10 | Skc株式会社 | 双波长反射多层膜 |
CN105899977A (zh) * | 2013-12-18 | 2016-08-24 | 柯尼卡美能达株式会社 | 光反射膜及使用该光反射膜的光反射体 |
CN105899977B (zh) * | 2013-12-18 | 2019-04-26 | 柯尼卡美能达株式会社 | 光反射膜及使用该光反射膜的光反射体 |
Also Published As
Publication number | Publication date |
---|---|
IL122244A0 (en) | 1998-04-05 |
US20010008700A1 (en) | 2001-07-19 |
US6368699B1 (en) | 2002-04-09 |
JP2008162289A (ja) | 2008-07-17 |
CN1195317A (zh) | 1998-10-07 |
KR19990028380A (ko) | 1999-04-15 |
MX9710372A (es) | 1998-03-29 |
JP4122057B2 (ja) | 2008-07-23 |
KR100468560B1 (ko) | 2005-08-04 |
JPH11508706A (ja) | 1999-07-27 |
AU6390396A (en) | 1997-01-30 |
EP1537992A2 (en) | 2005-06-08 |
EP1537992A3 (en) | 2011-12-28 |
US6459514B2 (en) | 2002-10-01 |
BR9609314A (pt) | 1999-07-06 |
CA2222511A1 (en) | 1997-01-16 |
EP0836554A1 (en) | 1998-04-22 |
WO1997001440A1 (en) | 1997-01-16 |
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