CN1117995C - 一种光学薄膜 - Google Patents
一种光学薄膜 Download PDFInfo
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Abstract
提供一种光学薄膜,它包括设置在连续双折射基质中的聚合物颗粒的分散相。通过在一个或多个方向上进行拉伸使薄膜定向。选择分散相颗粒的大小和形状、分散相的容积分数、薄膜厚度以及定向量,以获得所需波长的电磁辐射在所得的薄膜中产生所需程度的漫反射和总透射。
Description
发明领域
本发明涉及含有适合控制光学性质如反射和透射的结构的光学材料。另一方面,本发明涉及控制反射光或透射光的具体偏振方向的方法。
背景
由掺杂物分散在连续基质中而制成的光学薄膜是本领域已知的。可通过控制这些掺杂物的特征来为薄膜提供一定范围的反射性和透射性。这些特征包括薄膜中掺杂物相对于波长的大小、掺杂物的形状和排列方式、掺杂物的体积填充因子(volumeric fill factor)和沿薄膜三个正交轴上掺杂物与连续基质的折射率不匹配程度。
传统的吸收(二向色性)偏振器有吸收光的无机杆状碘链排列在聚合物基质中作为偏振器的掺杂相。这种薄膜易于吸收电场矢量平行于杆状碘链的偏振光,并且易于透射电场矢量垂直于杆的偏振光。因为碘链有两个或更多个线度相对于可见光波长很小,而且每立方光波长中的链数目很大,所以这种薄膜的光学性质主要是镜面反射,而只有很少通过薄膜的漫透射或在薄膜表面的漫反射。和其它大多数商业上可获得的偏振器一样,这种偏振薄膜是以偏振选择性吸收为基础的。
填充有不同特性的无机掺杂物的薄膜可提供其它光学透射和反射性质。例如,在聚合薄膜和涂料中加入有两个或多个线度比可见光波长大的有涂层的云母薄片,以提供一种金属光泽。可设法将这些薄片放在薄膜平面内,从而为反射外观提供强的方向依赖性。这种效果可用来生产在某些视角高度反射而对其它视角透射的安全屏(securityscreen)。在薄膜中可加入有显色作用(镜面选择性反射)的大薄片(显色与薄片相对人射光的排列方式有关),以提供填充的证明(evidence oftampering)。在这种应用中,薄膜中的所有薄片必须以相同方式排列。
然而,用填充有无机掺杂物的聚合物制得的光学薄膜存在各种问题。一般来说,无机颗粒和聚合物基质间的粘合性差。因此,当应力或应变施加在基质上时,薄膜光学性质变差,这是由于基质和掺杂物间的结合被损害,而且刚性无机掺杂物可能破碎。而且,使无机掺杂物取向所需的加工步骤和考虑因素使生产变复杂。
其它薄膜,如美国专利4,688,900(Doane等)中公开的,包括一个透明的透射光的连续聚合物基质,其中分散有调制光的液晶滴。据报道,对这种材料进行拉伸,可使液晶滴从球形变形成椭球形,椭球体的长轴与拉伸方向平行。美国专利5,301,041(Konuma等)公开了相近的内容,但是液晶滴的变形是通过加压来实现的。A.Aphonin在《液晶》第19卷第4期469-480页的“分散有液晶的拉伸聚合物膜的光学性质:角度依赖的偏振光散射”(“Optical Properties of Stretched PolymerDispersed Liquid Crystal Flims:Angle-Dependent Polarized LightScattering,Liquid Crystals,Vol.19,No.4,469-480(1995))中讨论了聚合物基质内有液晶滴的拉伸过的薄膜的光学性质。他报道说,液滴拉长成长轴与拉伸方向平行的椭球形,使液滴具有取向双折射性(液滴各轴上折射率不同),从而导致沿薄膜某一轴上分散相和连续相间折射率相对地不匹配,而沿薄膜其它轴上折射率相对地匹配。这种液晶滴并不比薄膜内的可见光波长小,因此这种薄膜的光学性质是它们的反射和透射性质中有很大的漫射成分。Aphoni建议用这些材料作为背后照明扭曲向列型LCD(backlit twisted nematic LCD)的偏振漫射器。然而,用液晶作为分散相的光学薄膜严重地受到基质相和分散相间折射率不匹配的程度的限制。而且,这种薄膜的液晶成分的双折射性通常对温度敏感。
美国专利5,268,225(Isayev)公开了从热致的液晶聚合物的混合物制得的复合层压片。混合物包括两种互不相溶的液晶聚合物。混合物可流延成含有一分散的掺杂相和一连续相的薄膜。在拉伸薄膜时,分散相形成了其轴排列在拉伸方向上的一系列纤维。尽管据说薄膜有改善的机械性能,但是没有提到薄膜的光学性质。然而,由于它们的液晶特点,这种类型的薄膜将遇到上述其它液晶材料所遇到的问题。
还有其它在施加电场或磁场时呈现所需光学性质的薄膜。例如,美国专利5,008,807(Waters等)描述了一种液晶装置,它含有一层用液晶材料渗透的且位于两个电极之间的纤维。电极之间的电压产生一个电场,改变了液晶材料的双折射性,从而导致纤维和液晶的折射率间不同程度的折射率不匹配。然而,需要用电场或磁场是不方便的,并且在许多应用场合是不希望的,特别是那些存在的场会产生干扰的场合。
还有的其它光学薄膜是将第一聚合物作为掺杂分散物加入第二聚合物中,然后在一个或两个方向上拉伸得到的复合体来制得。美国专利4,871,784(Otonari等)是这种技术的代表。聚合物选择得使分散相和周围基质聚合物间的粘合性较差,使得在拉伸薄膜时在每个掺杂物周围形成椭球形空隙。这种空隙的尺寸与可见光波长大致相当。在这些有“微空隙”的薄膜中,空隙和聚合物间的折射率不匹配通常相当大(约为0.5),从而引起大量漫反射。然而,由于界面的几何结构不同,所以微空隙材料的光学性质很难控制,而且不能形成折射率相当匹配的薄膜轴,而折射率相当匹配的轴对于偏振敏感的光学的质是有用的。另外,这些材料中的空隙在暴露在热和压力下时很容易瘪塌。
也制成了分散相以有序的方式确定地排列在连续基质中的光学薄膜。美国专利5,217,794(Schrenk)是这种技术的代表,其中公开了一种用聚合掺杂物制成的层状聚合薄膜,掺杂物在两个轴上的尺寸比波长大,它排列在另一聚合材料的连续基质中。分散相沿层压片一个或更多个轴向的折射率与连续相折射率明显不同,而在另一方向上相当匹配。由于分散相的有序化(ordering),因此这种类型的薄膜在它们主要是反射的情况下表现出很强的虹彩(即以干涉为基的与角度有关的显色(interference-based angle dependent coloring))。因此,在希望有光学漫射的场合下,这种薄膜的用途有限。
因此,本领域中需要一种光学材料,它包括一连续相和一分散相,其中可对材料在三维轴向上两相间的折射率不匹配进行方便而持久的控制,以获得所需程度的漫射、镜面反射和透射,其中光学材料对于应力、应变、温度差异以及电场和磁场是稳定的,其中光学材料有低水平的虹彩。本发明,如下面所公开的,满足了这些以及其它要求。
附图简述
图1表示根据本发明制得的光学体,其中分散相排列成一系列截面基本为圆形的伸长物;
图2表示根据本发明制得的光学体,其中分散相排列成一系列截面基本呈椭圆形的伸长物;
图3a-e表示根据本发明制得的光学体中分散相的各种形状;
图4a是本发明的取向薄膜中垂直于取向方向的偏振光的双向散射分布与散射角度的关系;
图4b是本发明的取向薄膜中平行于取向方向的偏振光的双向散射分布与散射角度关系;和
图5表示根据本发明制得的多层薄膜。
发明概要
本发明一方面涉及一种漫反射薄膜或其它光学体,它包含双折射连续聚合物相和排列在连续相中的基本上非双折射的分散相。连续相和分散相的折射率在三个相互正交轴的第一个轴向上是基本不匹配的(即,相互之间的差大于约0.05)。而在三个相互正交轴的第二个轴向上是基本匹配的(即,差异小于约0.05)。在一些例子中,连续相和分散相的折射率沿或平行于三个相互正交轴的第三个轴向上是基本匹配或不匹配的,以制成反射镜或偏振器。沿或平行于不匹配轴偏振的人射光被散射,从而导致了显著的漫反射。沿匹配轴偏振的入射光被散射的程度要低得多,它主要是镜面透射(spectrally transmitted)。这些性质可用来制备各种用途的光学薄膜,包括用来漫反射没有被显著地透射的偏振光的低损失(没有显著的吸收)反射偏振器。
本发明的一个相关方面涉及一种光学薄膜或其它光学体,它包含一双折射连续相和一分散相,其中连续相和分散相的折射率在垂直于光学体表面的轴向上是基本匹配的(即,其中连续相和分散相的折射率差小于约0.05)。
本发明另一方面涉及一种组合的光学体,它包含一聚合物双折射连续相(第一相),其中的分散相(第二相)可以是双折射的,但是至少两个正交方向上的匹配和不匹配程度主要是由第一相的双折射引起的。
本发明还有一个方面涉及一种获得漫反射偏振器的方法,包括以下步骤:提供第一种树脂,它的双折射程度可通过施加一个力场(如通过空间取向而产生的)或施加一个电场来改变,从而使获得的树脂材料在至少两个正交方向上的折射率之差大于约0.05;提供第二种树脂,使其分散在第一种树脂中;和向两个树脂的复合体施加所述力场,使得两种树脂的折射率在两个方向中的一个方向上大致匹配,相差小于约0.05,而在两个方向中的另一个方向上,第一种和第二种树脂间折射率差大于约0.05。在一个相关的例子中,是在施加力场从而改变第一种树脂的双折射性后,将第二种树脂分散在第一种树脂中。
本发明还有一个方面涉及一种作为高消光比反射偏振器的光学体。在这个方面,匹配方向上的折射率差应选得尽可能小,而不匹配方向上的折射率差应尽可能大。体积分数、厚度和分散相颗粒大小和形状的选择应使消光比最大,尽管对于不同的应用,不同偏振态的光学透射和反射的相对重要性有所不同。
本发明另一个方面涉及一种光学体,它包含一个连续相,一个分散相和一种二向色性染料,分散相的折射率与所述连续相不同,它们间的差在第一轴向上大于约0.05,在正交于所述第一轴向的第二轴向上小于约0.05。光学体最好沿至少一个轴向取向。二向色性染料通过吸收(除散射外)平行于取向轴偏振的光提高了光学体的消光系数。
本发明另一个方面涉及一种光学体,其特征在于:所述第一与第二相的折射率之差的绝对值沿第一轴为Δn1而沿正交于所述第一轴的第二轴为Δn2,这里,Δn1与Δn2之差的绝对值至少约为0.05,这里,对于电磁辐射的至少一种偏振方向,所述第一和第二相沿至少一个轴一起获得的漫反射率至少约为30%。
本发明另一个方面涉及一种光学体,该光学体为一种偏振片。
在本发明的各个方面,通过选择或控制各种参数,包括连续相和分散相的光学折射率、分散相颗粒的大小和形状、分散相的体积分数、部分入射光通过的光学体的厚度和感兴趣的电磁辐射波长或波段(wavelength band),可确定入射光的至少两个正交偏振的反射和透射性质。
沿一特定轴向的折射率匹配或不匹配的大小将直接影响沿该轴偏振的光的散射程度。通常,散射本领与折射率不匹配的平方成正比。因此,沿一特定轴的折射率不匹配越大,沿该轴偏振的光的散射就越强。相反,当沿一特定轴的不匹配很小时,沿该轴偏振的光的散射程度就很小,从而镜面透射通过整个物体。
分散相的大小对散射也有显著影响,如果分散相颗粒太小(即,小于媒质内感兴趣光波长的约1/30),且每立方波长内有许多颗粒的话,光学体就相当于一个沿任何给定轴的有效折射率在两个相的折射率之间的媒质。在这种情况下,很少有光散射。如果颗粒太大,则光从颗粒表面镜面散射,很少有光漫射至其它方向。当颗粒在至少两个正交方向上太大时,也会发生不希望有的虹彩效应。当颗粒变大时也会到达实际生产的极限,因为光学体的厚度会变大,而所需的机械性质会受到损害。
分散相颗粒的形状也会影响光散射。颗粒对折射率匹配和不匹配方向上的电场消偏振系数会减少或增加给定方向上的散射量。其效果会增强或减弱(detract)折射率不匹配产生的散射量,但是在本发明中的性质较佳范围内,其对散射的影响通常很少。
颗粒的形状也影响从颗粒散射出的光的漫射程度。这种形状影响通常是很小的,但是随着垂直于入射光方向的平面中颗粒几何截面的纵横比增加和颗粒变得相对较大,这种影响会增加。通常,在实施本发明时,如果希望是漫反射而不是镜面反射,那么分散相颗粒在一个或两个互相正交方向上的大小应小于数个光波长。
分散相的空间排列对散射能力也有影响。特别发现,在本发明制得的光学体中,经排列的散射体不会象随机排列的散射体那样绕镜面透射或反射方向的对称地散射光,特别地,通过取向被拉成杆状的掺杂物基本上沿着以取向方向为中心且边缘沿镜面透射方向的圆锥(或附近)散射光。例如,对于从垂直于取向的方向入射到这种拉长杆上的光,散射光呈现为在垂直于取向方向的平面内的一条光带,其强度随着离开镜面方向的角度增加而减弱。通过调节掺杂物的几何结构,可对散射光在透射半球和反射半球中的分布进行一定的控制。
分散相的体积分数也对本发明光学体中的光散射有影响。在一定的范围内,增加分散相的体积分数会增加光线进入物体后在匹配和不匹配方向上偏振光发生的散射量。这一因素对于控制给定应用场合下的反射和透射性质是重要的。然而,如果分散相的体积分数太大,则光散射会减小。不拟与理论结合,这看来是由于分散相颗粒相对于光波长来说靠得太近,从而各颗粒的共同作用,相当于数量较少的等效大颗粒。
光学体的厚度也是一个重要的控制参数,可通过控制它来影响本发明中的反射和透射性质。随着光学体厚度的增加,漫反射也会增加,而镜面透射和漫透射都会减弱。
尽管本发明是参照光谱的可见区域来进行描述的,但是通过适当地按比例改变光学体的组分,本发明的各种例子可用于电磁辐射的不同波长(以及频率)。因此,随着波长的增加,光学体组分的线度应增加,使得尺度(以波长单位测定)大约保持恒定。改变波长的另一个主要影响是,对于大多数感兴趣的材料来说,折射率和吸收系数的变化。然而,折射率匹配和不匹配的原理仍适用于每一种感兴趣的波长。发明详述导论
本文中,术语“镜面反射”指光线反射至以镜面角为中心、顶角为16°的出射圆锥体内。术语“漫反射”指光线反射至上述镜面反射圆锥体外。术语“总反射”指表面上所有光线的总的反射。因此,总反射是镜面反射和漫反射之和。
同样,本文所用的术语“镜面透射”指光线透射至以镜面方向为中心、顶角为16°的出射圆锥体内。本文所用的术语“漫透射”指光线透射至上述镜面透射圆锥体外。术语“总透射”指透射通过光学体的所有光线的总和。因此,全透射是镜面透射和漫透射之和。
本文所用的术语“消光比”定义为在一个偏振方向下透过的光的总量与正交偏振方向下透过的光之比。
图1-2描述了本发明的第一个例子。根据本发明制得漫反射性光学薄膜10或其它光学体,它包括一个双折射性基质即连续相12和一个不连续或分散相14。连续相的双折射性通常至少约为0.05,更佳的至少约为0.1,还要佳的至少为约0.15,最佳的至少约为0.2。
连续相和分散相的折射率沿三个互相正交轴中第一个轴是基本匹配的(即,折射率差小于约0.05),且沿三个互相正交轴中第二个轴是基本上不匹配的(即,其差大于约0.05)。较佳的,在匹配方向上连续相和分散相的折射率差小于约0.03,小于约0.02更佳,小于约0.01最佳。在不匹配方向上连续相和分散相的折射率差宜至少约为0.07,更佳的应至少约为0.1,最佳的应至少约为0.2。
沿一特定轴的折射率不匹配的效果是,沿该轴偏振的入射光基本上被散射,从而形成显著数量的反射。相反,沿折射率匹配的轴方向偏振的入射光会镜面透射或镜面反射,而只有很少程度的散射。这个效果可用来制备各种光学器件,包括反射偏振器和反射镜。
本发明的光学体对于电磁辐射的至少一种偏振方向,所述第一和第二相沿至少一个轴一起获得的漫反射率至少约为30%,优选约为50%。对于所述的电磁辐射的第一偏振方向,所述光学体的总反射率大于50%;对于电磁辐射的正交于所述第一偏振方向的第二偏振方向,所述光学体的总透射率大于50%。至少有40%的以正交于光束的第一光偏振方向偏振的光以小于8°的偏转角透过所述的光学体。
本发明的光学体,对于可见光、紫外或红外电磁辐射的至少一个偏振方向,所述第一和第二相沿至少一个轴向一起获得的漫反射率至少为30%。至少有40%的正交于光束的第一偏振方向的偏振光漫射透过所述光学体;所述的漫透射光线主要分布在圆锥表面上或其附近,圆锥表面包含镜面透射方向而圆锥轴以拉伸方向为中心。
本发明提供了一种实用而简单的光学体,和制备一种反射偏振器的方法,也提供了一种根据本文所述原理获得连续范围的光学性质的方法。同样,也可获得非常有效的低损失高消光比偏振器。其它优点是有广泛的实用材料用于分散相和连续相,以及在提供有稳定而可预测的高质量性能的光学体时有高度的控制性。折射率匹配/不匹配的效果
在较佳的例子中,连续相和分散相中的至少一种材料是一种在取向时折射率发生改变的材料。所以,当薄膜在一个或多个方向上取向时,沿一个或多个轴产生了折射率匹配或不匹配。通过仔细控制取向参数和其它加工条件,基质的正或负双折射性可用来产生沿一个或两个给定轴偏振的光的漫反射或漫透射。透射和漫反射间的相对比例取决于分散相掺杂物的浓度、薄膜厚度、连续相和分散相间的折射率差的平方、分散相掺杂物的大小和几何形状以及入射辐射的波长或波段。
沿一特定轴的折射率匹配或不匹配的量值直接影响沿该轴偏振的光的散射程度。通常,散射本领随折射率不匹配的平方变化。因此,沿一特定轴的折射率不匹配越大,沿该轴的偏振光散射就越强。相反,当沿一特定轴的不匹配很小时,沿该轴偏振的光散射的程度就很小,从而镜面透射通过物体。
图4a-b说明了根据本发明制得的取向薄膜中的这个效果。其中显示了632.8nm的法向入射光的典型的双向散射分布函数(BidirectionalScatter Distribution Function)(BSDF)测定结果。BSDF在J.Stover的“光学散射测量和分析”(“Optical Scattering Measurement and Analysis”)(1990)中有所描述。这两个图显示了垂直和平行于取向轴的偏振光的BSDF与散射角的关系。0°散射角与末散射(镜面透射)光对应。对于在折射率匹配方向(即,与取向方向垂直的方向)上的偏振光来说,如图4a中所示,有一个明显的镜面透射峰,并有相当多的漫透射光(散射角在8至80°间),以及少量漫反射光(散射角大于100°)。而对于在折射率不匹配方向(即,与取向方向平行的方向)上的偏振光来说,如图4b所示,有可忽略的镜面透射光和数量大大减少的漫透射光,和相当多的漫反射光。应当注意的是,这些曲线表示的散射平面是与这些伸长掺杂物的取向方向垂直的平面(大多数散射光在这个平面内)。在该平面外的散射光则大大减弱。
如果掺杂物(即分散相)沿某一轴的折射率与连续的主体媒介匹配,那么电场与该轴平行的入射偏振光将通过而不散射,不论掺杂物的大小、形状和密度如何。如果沿某一轴的折射率不匹配,那么掺杂物将散射沿该轴偏振的光。对于有给定截面积、线度大于约λ/30(λ是媒介中光的波长)的散射体,散射强度在很大程度上由折射率不匹配值来决定。不匹配掺杂物的确切大小、形状和排列方式在决定有多少光从该掺杂物散射到各方向上起一定作用。如果散射层的密度和厚度足够大,根据多重散射理论,入射光会被反射或吸收,而不会透射,无论散射体的具体大小和形状如何。
当材料被用作偏振器时,它最好通过拉伸处理,并允许平面内拉伸方向的横向上有一定的尺寸松弛,使沿平行于材料表面的平面内第一轴的连续相和分散相间折射率差较大而沿其它两个正交轴较小。这就导致了对不同偏振,的电磁辐射有较大的光学各向异性。
本发明范围内的一些偏振器是椭圆偏振器。通常,椭圆偏振器在拉伸方向和拉伸方向的横向上均存在分散相和连续相间的折射率差。前向和反向散射之比依赖于分散相和连续相间的折射率差、分散相的浓度、分散相的大小和形状以及薄膜的总厚度。通常,椭圆漫射体中分散相颗粒和连续相间的折射率差比较小。通过使用以双折射性聚合物为基的漫射体,可获得高度的椭圆偏振灵敏度(即,漫反射率依赖于光的偏振方式)。在极端情况下,当聚合物的折射率在一个轴上匹配时,椭圆偏振器将是一种漫反射偏振器。获得折射率匹配/不匹配的方法
用于本发明的偏振器的材料,以及这些材料的取向程度最好选择成使得,在制成的偏振器中,两个相至少在一个轴上的相关折射率是基本相等的。该轴(它通常是,但不是必须是,取向方向的横向)上的折射率匹配会导致在该偏振平面上基本没有光反射。
在拉伸后,分散相在取向方向上的折射率也会有所降低。如果主体的双折射性是正型(Positive)的,则分散相具有负型(negative)应变诱导的双折射性时,有提高取向轴上相邻相之间折射率差的优点,尽管偏振平面与取向方向垂直的光的反射仍是可忽略的。在取向后,取向方向的正交方向上相邻相间的折射率差应小于约0.05,最好小于约0.02。
分散相也可表现出正型应变诱导的双折射性。所述第二分散相的双折射小于约0.02,优选小于约0.01。然而,这可通过热处理来改变,以使垂直于连续相取向方向的轴上的折射率匹配。热处理温度不应过高而使连续相中的双折射性松弛(relax)。
所述第二分散相的折射率不同于所述第一连续相的折射率,沿一个第一轴方向其折射率差为大于约0.1,大于约0.15更好,大于约0.2最好。而沿正交于第一轴的所述第二轴方向其折射率差为小于约0.03,小于约0.01更好。分散相的大小
分散相的大小对散射也有显著影响。如果分散相颗粒太小(即,小于感兴趣的光在媒质内波长的约1/30),且每立方波长内有许多颗粒的话,光学体就相当于一个沿任何给定轴的有效折射率在两个相的折射率之间的媒质。在这种情况下,很少有光散射。如果颗粒太大,则光从颗粒表面镜面散射,很少有光漫射至其它方向。当颗粒在至少两个正交方向上太大时,也会发生不希望有的虹彩效应。当颗粒变大时也会到达实际生产的极限,因为光学体的厚度会变大,而所需的机械性质会受到损害。
在排列后,分散相颗粒的尺寸可根据光学材料所要求的用途而不同。因此,例如,颗粒的尺寸可根据具体应用中的感兴趣的电磁辐射波长而不同,对于反射或透射可见光、紫外线、红外线和微波辐射,需要有不同的尺寸。然而,通常颗粒的长度应约大于媒质中感兴趣的电磁辐射波长的1/30。
较佳地是,在光学体用作低损失反射偏振器时,颗粒的长度约大于感兴趣波长范围内电磁辐射波长的2倍,最好大于波长的4倍。颗粒的平均直径宜等于或小于感兴趣波长范围内的电磁辐射波长,最好小于所持波长的0.5倍。尽管分散相的尺寸在许多应用中是次要的考虑因素,但是在漫反射相对较少的薄膜应用中,它变得较为重要。分散相的几何形状
尽管折射率不匹配是本发明薄膜中赖以促进散射的主要因素(即,根据本发明制得的漫射镜或偏振器在至少一个轴上连续相和分散相的折射率有明显不匹配),但是分散相颗粒的几何形状对于散射有次要的影响作用。因此,颗粒对折射率匹配和不匹配方向上的电场的退极化因子可减少和增加给定方向上的散射量。例如,当分散相在沿垂直于取向轴的平面上截取的截面是椭圆形时,分散相的椭圆形截面形状会在反向散射光和前向反射光中产生不对称漫射。该影响可增强或减强(detract)由折射率不匹配产生的散射量,但是在本发明较佳的性质范围内,其对散射的影响较小。
分散相颗粒的形状也影响从颗粒散射出的光的漫射程度。这种形状的影响通常是很小的,但是随着垂直于入射光方向的平面中颗粒几何截面的纵横比增加和颗粒变得相对较大,这种影响会增加。通常,在实施本发明时,如果希望是漫反射而不是镜面反射,那么分散相颗粒在一个或两个互相正交方向上的大小应小于数个光波长。
对于低损失反射偏振器来说,较佳的例子中包括位于连续相中的一系列杆状结构的分散相,该结构经取向而有较高的纵横比,该纵横比可通过提高平行于取向方向的偏振光相对于垂直于取向方向的偏振光的散射强度色散来提高其反射。然而,如图3a-e所示,分散相可以有许多不同的几何结构。因此,分散相可以是碟状或伸长的碟状(如图3a-c所示)、杆状(如图3d-e所示)或球状的。其它可考虑的例子是,其中分散相截面积大致呈椭圆形(包括圆形)、多边形、不规则形状或这些形状的一个或多个的组合。分散相颗粒的截面形状和大小可以随不同颗粒而不同、或随不同薄膜区域(即,从表面到芯部)而不同。
在一些例子中,分散相可以有一芯壳结构,其中芯和壳可用相同或不同的材料制成,或者芯是中空的。因此,例如,分散相可包含长度相等或随机的、截面均一或不均一的中空纤维。纤维的内部空间可以是空的,或可被固体、液体或气体、有机或无机的合适媒质占据。该媒质的折射率可根据分散相和连续相的折射率来选择,以获得所需的光学效应(即,沿一给定轴的反射或偏振)。
通过对光学材料适当地取向或加工、采用有特定几何结构的颗粒或两者的组合,可获得分散相所需的几何结构。因此,例如,基本呈杆状结构的分散相可通过使含有大致呈球形的分散相颗粒的薄膜沿一个轴取向来制备。通过对薄膜在垂直于第一个轴的第二方向上取向,杆状结构可获得椭圆形截面。作为另一个实施例,基本上是杆状结构,且杆的截面积是矩形的分散相可通过将一个其中的分散相含有一系列基本上为矩形的薄片的薄膜在一个方向取向来制得。
拉伸是一种获得所需几何结构的简便方法,因为拉伸也可用来使材料内的折射率产生差异。如上所述,根据本发明制得的薄膜可以在多个方向上取向,并且可以相继地或同时进行。对所述的光学体进行拉伸的拉伸比至少约为2至6。
在另一个实施例中,连续相和分散相的组分可被挤塑,使得分散相在末取向薄膜中的一个轴上呈杆状。通过在挤塑薄膜中杆的主轴方向上取向,可获得有较高纵横比的杆。通过在挤塑薄膜中杆主轴的正交方向上取向,可获得片状结构。
图2中的结构可通过对连续基质中基本呈球形的颗粒混合物进行不对称双轴取向来制得。或者,结构可通过将多个纤维状结构加入基质材料中,便结构沿一个轴排列并使混合物在该轴横向上取向来制得。获得这种结构的还有一种方法是,控制聚合物混合物中各组分的相对粘度、剪切力或表面张力,以在混合物挤塑成薄膜时产生纤维状分散相。通常,在挤塑方向上施加剪切力时可获得最好的效果。分散相的空间排列
空间排列也对分散相的散射能力有影响。特别发现,在本发明制得的光学体中,经排列的散射体不会象随机排列的散射体那样绕镜面透射或反射方向对称地散射光。特别地,通过取向被拉成杆状的掺杂物基本上沿以取向方向为中心并沿镜面透射方向的圆锥表面(或附近)散射光。这会导致散射光在镜面反射和镜面透射方向周围的各向异性分布。例如,对于垂直取向的方向入射到这种拉长杆上的光来说,散射光呈现为垂直于取向方向的平面上的光带,其强度随着离开镜面方向的角度增加而减弱。通过调节掺杂物的几何结构,可对散射光在透射半球和反射半球中的分布进行一定的控制。分散相的尺寸
在光学体用作低损耗反射偏振器的应用中,分散相的结构最好有高的纵横比,即结构的一个线度比其它所有线度大得多。纵横比宜至少为2,更佳地至少为5。最大线度(即长度)宜至少为感兴趣波长范围内电磁辐射波长的2倍,更佳的至少为所需波长的4倍。另一方面,分散相结构的较小(即截面线度)宜小于或等于感兴趣的波长,更佳的应小于感兴趣波长的0.5倍。分散相的体积分数
分散相的体积分数也对本发明光学体中的光散射有影响。在一定的范围内,增加分散相的体积分数会增加光线进入物体后在匹配和不匹配方向上的偏振光发生的散射量。这一因素对于控制给定应用场合下的反射和透射性质是重要的。然而,如果分散相的体积分数太大,则光散射会衰减。不拟与理论结合,这看来是由于分散相颗粒相对于光波长来说靠得太近,因而各颗粒的共同作用,相当于数量较少的等效大颗粒。
所需的分散相体积分数依赖于多种因素,包括连续相和分散相材料的具体选择。然而,通常分散相的体积分数至少约为连续相的1%(体积),更佳的在约5至15%范围内,最佳的在15至30%范围内。光学体的厚度
光学体的厚度也是一个重要的参数,可通过控制它来影响本发明的反射和透射性质。随着光学体厚度的增加,漫反射也会增加,而镜面透射和漫透射会减弱。因此,尽管光学体的厚度通常选择成使最终产物具有所需的机械强度,但是它也可用来直接控制反射和透射性质。
也可用厚度来最终调节光学体的反射和透射性质。因此,例如在薄膜涂布中,用来挤塑薄膜的装置可由测定挤塑薄膜中的透射和反射值、改变薄膜厚度(即通过调节挤塑速率或改变流延轮速度(castingwheel speed)来改变)的下游光学装置来控制,以使反射和透射值保持在预定的范围内。连续相/分散相的材料
根据光学体涉及的具体应用,许多不同的材料可用作本发明光学体的连续相或分散相。这些材料包括无机材料如二氧化硅为基的聚合物、有机材料如液晶,以及聚合材料、包括单体、共聚物、接枝聚合物、及它们的混合物。给定应用中材料的准确选择是由特定轴上连续相和分散相间所希望得到的折射率匹配和不匹配、以及获得产品中所需的物理性质决定的。然而,连续相材料的特征通常是其在所需光谱区域下是基本上透明的。
在选择材料时另一个考虑因素是,得到的产品必须含有至少两个不同的相。这可通过浇铸从两种或多种互不混溶的材料获得的光学材料来实现。或者,如果需要用相互混溶的第一和第二种材料制备光学材料,且第一种材料的熔点比第二种材料高的话,在一些情况下可以在低于第一种材料熔点的温度下将尺寸合适的第一种材料颗粒包埋在第二种材料的熔融基质中。然后得到的混合物可以流延成薄膜,随后取向或不取向,制成光学器件。
适于用作本发明中的连续相或分散相的聚合材料可以是非晶形、半晶形、或结晶的热塑性树脂聚合材料,包括从基于羧酸(如间苯二酸、壬二酸、己二酸、癸二酸、二苯甲酸(dibenzoic acid)、对苯二甲酸、2,7-萘二甲酸、2,6-萘二甲酸、环己烷二羧酸和联苯甲酸(包括4,4’-联苯甲酸))的单体制得的材料,或从上述酸的相应酯(即,对苯二甲酸二甲酯(dimethylterephthalate))制得的材料。其中,聚-2,6-萘二甲酸乙二醇酯(PEN)(2,6-polyethylene naphthalate)是特别佳的,因为它有应变诱导双折射性和在拉伸后持久保持双折射性的能力。PEN对于波长为550nm的入射偏振光,当偏振平面与拉伸轴平行时,其折射率在拉伸后从约1.64升高至高达约1.9,而对于垂直于拉伸轴偏振的光,其折射率是降低的。PEN在可见光谱内双折射为0.25至0.40(在这种情况下,是沿拉伸方向的折射率和垂直于拉伸方向折射率之差)。双折射可通过提高分子取向来增加。根据制备薄膜时所用的加工条件,PEN在约155℃至高达约230℃下基本上是热稳定的。
聚萘二甲酸丁二醇酯以及其它结晶萘二甲酸聚酯也是合适的材料。结晶萘二甲酸聚酯在平面内不同轴上的折射率差至少为0.05,最好大于0.20。
当用PEN作为本发明光学材料中的一个相时,另一个相宜为聚甲基丙烯酸甲酯(PMMA)或间规立构乙烯基芳族聚合物如聚苯乙烯(sPS)。其它与PEN一起使用的较佳聚合物是基于对苯二甲酸、间苯二酸、癸二酸、壬二酸或环己烷二羧酸或这些物质相应的烷基酯的聚合物。也可用少量的萘二甲酸来改善相间的粘合性。二醇组分可以是乙二醇或相关的二醇。较佳的,所选聚合物的折射率小于约1.65,更佳的小于约1.55,虽然使用有更高折射率的聚合物可获得相同的结果,如果有相同的折射率差的话。
用于本发明的间规立构乙烯基芳族聚合物包括聚(苯乙烯)、聚(烷基苯乙烯)、聚(苯乙烯卤化物)、聚(烷基苯乙烯)、聚(苯甲酸乙烯酯)及其氢化的聚合物和混合物,或含有这些结构单元的共聚物。聚(烷基苯乙烯)的例子包括:聚(甲基苯乙烯)、聚(乙基苯乙烯)、聚(丙基苯乙烯)、聚(丁基苯乙烯)、聚(苯基苯乙烯)、聚(乙烯基萘)、聚(乙烯基苯乙烯)和聚(苊)。聚(苯乙烯卤化物)的例子包括:聚(氯苯乙烯)、聚(溴苯乙烯)和聚(氟苯乙烯)。聚(烷氧基苯乙烯)的例子包括:聚(甲氧基苯乙烯)和聚(乙氧基苯乙烯)。在这些例子中,特别佳的苯乙烯基团聚合物是:聚苯乙烯、聚(对甲基苯乙烯)、聚(间甲基苯乙烯)、聚(对叔丁基苯乙烯)、聚(对氯苯乙烯)、聚(间氯苯乙烯)、聚(对氟苯乙烯),以及苯乙烯和对甲基苯乙烯的共聚物。
另外,除了上述苯乙烯基团聚合物的单体外,作为间规立构乙烯基-芳族基团共聚物的共聚单体还有烯烃单体如乙烯、丙烯、丁烯、己烯或辛烯;二烯烃单体如丁二烯、异戊二烯;极性乙烯基单体如环二烯单体、甲基丙烯酸甲酯、马来酸酐或丙烯腈。
本发明的间规乙烯基芳族聚合物可以是嵌段共聚物、无规共聚物或交替共聚物。
本发明中所指的有高水平间规结构的乙烯基芳族聚合物通常包括间规规正度高于75%(用C-13核磁共振测得)的聚苯乙烯。较佳的,间规规正度应高于85%外消旋二单元体(diad),或高于30%外消旋五单元体(pentad),较佳的应高于50%。
另外,尽管没有具体限制这些间规-乙烯基芳族基团聚合物的分子量,但是其重均分子量宜大于10000而小于1000000,更佳的应大于50000而小于800000。
关于其它树脂,可提到的各种类型,包括无规立构的乙烯基芳族基团聚合物、全同立构的乙烯基芳族基团聚合物,以及所有可混溶的聚合物。例如,聚亚苯基醚表现出良好的与前述乙烯基芳族基团聚合物的混溶性。而且,这些可混溶的树脂组分的成分宜在70至1%重量间,或更佳的在50至2%重量间。当可混溶树脂组分的成分超过70%,耐热性就会变差,而这通常是不希望的。
某一特定相的所选聚合物不必是共聚多酯或共聚碳酸酯。也可采用由乙烯基萘、苯乙烯、乙烯、马来酐、丙烯酸酯和甲基丙烯酸酯之类单体制得的乙烯基聚合物和共聚物。也可用非聚酯和聚碳酸酯之外的缩聚物。合适的缩聚物包括聚砜、聚酰胺、聚氨基甲酸乙酯、聚酰胺酸和聚酰亚胺。如果需要使折射率大致匹配,且PEN是主体的话,可用萘基团和卤素如氯、溴和碘来使所选聚合物的折射率增大到所需水平(1.59至1.69)。丙烯酸酯基团和氟对降低折射率特别有用。
可用少量的共聚单体代入萘二甲酸聚酯,只要取向方向上的大的折射率差基本不受损失。较小的折射率差(因此降低了反射性)可由下列任何优点弥补:连续相和分散相间的改善的粘合性、挤塑温度的降低和熔融粘度较好的匹配。光谱区域
尽管本发明通常是参照光谱的可见区域来进行描述的,但是通过适当地按比例改变光学体的组分,本发明的各个例子可用于不同的电磁辐射波长(以及频率)。因此,随着波长的增大,可增加光学体组分的线性大小,使得这些组分的尺寸(以波长单位测定)大致保持恒定。
当然,改变波长的一个主要影响是,对于大多数感兴趣的材料来说,折射率和吸收系数的变化。然而,折射率匹配和不匹配的原理仍适用于每一种感兴趣的波长,并可用来选择在特定光谱区域中操作的光学器件所用的材料。因此,例如,适当地按比例改变尺寸就可在光谱中红外区、近紫外区和紫外区中操作。在这种情况下,折射率指在这些操作波长下的数值,物体厚度和分散相散射成分的大小也应大致根据波长来按比例改变。可采用甚至更广的电磁波谱,其包括甚高频、超高频、微波和毫米波频率。这时仍存在根据波长适当按比例改变的偏振和漫射效应,折射率可从介电函数(dielectric function)(包括实部和虚部)的平方根获得。在这些波长较长的频带中,有用的产品可以是漫反射偏振器和部分偏振器。
在本发明的一些例子中,光学体的光学性质在感兴趣的波长频带范围内是不同的。在这些例子中,可用于连续相和/或分散相的材料,在一个或多个轴上的折射率在一个波长区域内与另一个区域是不同的。连续相和分散相材料的选择、材料具体选择后获得的光学性质(即,漫射和分散体反射或镜面透射)将依赖于感兴趣的波段。皮层
一层基本上没有分散相的材料可共同伸展置放在薄膜(即,分散相和连续相的挤塑混合物)的一个或两个主表面上。该层(也称作“皮层”)的组合物可以选择成,例如,用以保护分散相在挤塑混合物中的完整性,增加最终薄膜的机械或物理性质,或是在最终薄膜中增加光学功能,所选的合适材料包括连续相的材料或分散相的材料。熔融粘度与挤塑混合物相同的其它材料也是有用的。
皮层将使挤塑混合物在挤塑过程中,尤其是在模头可能会遇到的较宽的剪切强度范围变窄。高的剪切环境会引起不利的表面空隙并产生有纹路的表面。在薄膜厚度内有较宽范围的剪切值也会阻碍分散相在混合物中形成所需的颗粒大小。
皮层也会增加所得复合体的物理强度,或减少加工中的问题,例如减少薄膜在取向过程中撕裂的趋势。保持为非晶形的皮层材料易于制备韧性较高的薄膜,而半晶形的皮层材料则易于制备拉伸模量较高的薄膜。皮层中可加入其它功能性组分,如抗静电添加剂、紫外线吸收剂、染料、抗氧化剂和颜料,只要它们基本不不干扰制得产品所需的光学性质。
皮层可在挤塑过程中的某一时刻,即挤塑的混合物和皮层从挤塑模头中挤出之前,施加在挤塑混合物的一个或两个侧面上。这可采用传统的共挤塑方法来实现,该方法包括采用三层共挤塑模头。皮层也可以层压到挤塑混合物预先成型的薄膜上。总的皮层厚度为总混合物/皮层厚度的约2%至约50%。
有很多聚合物适于用作皮层。主要是非晶形的聚合物包括基于对苯二甲酸、2,6-萘二甲酸、间苯二酸、苯二酸、或它们的烷基酯对应物,以及亚烷基二醇,如乙二醇中的一种或多种的共聚多酯。半晶形聚合物的例子是聚-2,6-萘二甲酸乙二醇酯、聚对苯二甲酸乙二醇酯和尼龙材料。减反射层
根据本发明制备的薄膜和其它光学仪器也可含有一层或多层减反射层。这些层可以是偏振敏感或不敏感的,它们的作用是增加透射和减少反射光。一层减反射层可通过适当的表面处理方法,例如涂布或溅射蚀刻,施加到本发明的薄膜和光学器件上。
在本发明一些例子中,希望使透射最大和/或某些偏振光的镜面反射最小。在这些例子中,光学体可含有两层或多层,其中至少一层包含与提供连续相和分散相的层紧密接触的减反射系统。这种减反射系统的作用是减少入射光的镜面反射,增加进入包含连续和分散层的物体部分的入射光量。这种作用可通过该领域熟知的各种方法来实现。例子是四分之一波长减反射层、两层或多层减反射叠层(stack)、渐变折射率层和渐变密度层(graded density layer)。如果需要的话,这种减反射作用也可用于物体的透射光的一侧,以增强透射光。微空隙
在一些例子中,连续相和分散相的材料应选择得使两相间的界面足够薄弱,以便在薄膜取向时形成空隙。通过仔细控制加工参数和拉伸比、或选择性地使用相容剂,可以控制空隙的平均尺寸。最终产品中的空隙可用液体、气体或固体回填。空隙可与纵横比以及分散相和连续相的折射率结合起来产生作用,在制得的薄膜中获得所持的光学性质。两个以上的相
根据本发明制得的光学体也可包括两个以上的相。因此,例如,根据本发明制得的光学材料,其连续相中可包括两个不同的分散相。第二分散相可以随机或非随机地分散在整个连续相中,并可随机排列或是沿共同的轴排列。
根据本发明制得的光学体也可包括一个以上的连续相。因此,在一些例子中,除了第一连续相以及分散相外,光学体还可包括至少在一个方向上与第一连续相共同连续的第二相,在一个具体的例子中,第二连续相是一种与第一连续相共同伸展(即,第一连续相延伸通过伸展在第二连续相中的管道或空间网络中,就如水在湿海绵中通过管道网络结构一样)的海绵状的多孔材料。在一个相关的例子中,第二连续相具有枝状结构的形式,它在至少一个方向上与第一连续相共同伸展。多层组合
如果需要,可将一层或多层根据本发明制得的连续相/分散相薄膜组合使用,或是作为一多层薄膜的组分(即,用来增加反射)。合适的多层薄膜包括WO95/17303(Ouderkirk等)中所述的那些。在这样一个结构中,各个单独的层可以层压或是粘合在一起,或是分开的。如果薄层内相的光学厚度基本相同的话(就是说,如果两薄层沿一给定的轴对入射光表现出基本相等的大量散射体的话),复合体将会更有效地,大量反射与单独的薄层那相同的光谱范围和频带宽度(即,“频带”)内的光。如果层内相的光学厚度并不基本相等,那么复合体将会比单独层在更宽的频带中反射。镜面薄层与偏振器薄层组合而成的复合体可用来增加总反射率并仍能使透射光偏振。或者,单层可非对称地双轴取向,以制成有反射和偏振选择性的薄膜。
图5描述了本发明上述方式的一个实施例。其中,光学体是一个多层薄膜20,其中各层是PEN层22和co-PEN层24交替变化。每一PEN层包括一个在PEN基质中的间规聚苯乙烯(sPS)分散相。这类结构是所需的,因为它产生较低的偏离角色彩色(off-angle color)。另外,由于散射体层或其掺人使漏光量达到平衡,因此对于层厚度的控制就不那么关键,这使得薄膜更能容忍加工参数的变化。
前述的任何材料可用作本例子中的薄层、或作为特定层中的连续相或分散相。然而,PEN和co-PEN是特别合用的相邻层的主要组分,因为这些材料提供了良好的层间粘合性。
同样,在排列层时可有多种变化。因此,例如,各薄层可在结构的一部分或全部中按照重复顺序排列。其中一个例子是有…ABCABC…模式的结构,其中A、B和C是不同的材料、或相同或不同材料的不同混合物,并且A、B或C中的一个或多个含有至少一个分散相和至少一个连续相。皮层最好是相同或化学上相近的材料。添加剂
本发明的光学材料中也可含有其它本领域已知的材料或添加剂。这些材料包括颜料、染料、粘合剂、涂料、填充剂、相容剂、抗氧化剂(包括位阻酚)、表面活性剂、灭微生物剂、抗静电剂、阻燃剂、起泡剂、润滑剂、增强剂、光稳定剂(包括紫外线稳定剂或阻挡剂(blocker))、热稳定剂、撞击性能改良剂(impactmodifier)、增塑剂、粘度调节剂和其它材料。另外,根据本发明制备的薄膜和其它光学器件可包括一层或多层外表层,用来保护器件以防磨损、撞击或其它损伤,或是提高器件的加工性能或耐用性。
适用于本发明的润滑剂包括硬脂酸钙、硬脂酸锌、硬脂酸铜、硬脂酸钴、新十二烷酸钼(molybdenum neodocanoate)和乙酰丙酮酸钌(III)。
用于本发明的抗氧化剂包括4,4′-硫代双-(6-叔丁基-间甲酚)、2,2′-亚甲基双-(4-甲基-6-叔丁基丁酚)、3,5-二叔丁基-4-烃基氢化肉桂酸十八烷酯、双-(2,4-二叔丁基苯基)季戊四醇亚磷酸酯、IrganoxTM1093(1979)(膦酸((3,5-双(1,1-二甲基乙基)-4-羟基苯基)甲基)-十八烷基二酯)、IrganoxTM1098(N,N′-1,6-己二基双(3,5-双(1,1-二甲基)-4-羟基-苯丙酰胺)、NaugaardTM 445(芳胺)、IrganoxTM L57(二苯胺烷基化物)、IrganoxTM L115(含硫双酚)、IrganoxTM LO 6(苯基-δ-萘胺烷基化物(alkylated phenyl-delta-napthylamine))、Ethanox 398(氟代亚膦酸酯(flourophosphonite))、和2,2’-亚乙基双(4,6-二叔丁基苯基)氟代亚膦酸酯(2,2′-ethylidenebis(4,6-di-t-butylphenyl)fluorophosnite)。
特别佳的一组抗氧化剂是位阻酚,包括丁化羟基甲苯(BHT)、维生素E(二-α-生育酚)、IrganoxTM 1425WL(双-(O-乙基(3,5-二叔丁基-4-羟基苄基))磷酸钙)、IrganoxTM 1010(四(亚甲基(3,5,二叔丁基-4-羟基氢化肉桂酸酯))甲烷)、IrganoxTM 1076(3,5-二叔丁基-4-羟基氢化肉桂酸十八烷酯)、EthanoxTM 702(受阻双酚)、Etanox 330(高分子量受阻酚)、和EthanoxTM703(受阻酚胺)
二向色性染料是本发明光学材料的一些应用中特别有用的添加剂,因为当它们分子排列在材料中时,它们可吸收具有特定偏振的光。当其用于主要只散射一种偏振光的薄膜或其它材料时,二向色性染料可使材料对一种偏振光的吸收多于对另一种偏振光吸收。用于本发明的合适的二向色性染料包括刚果红(二苯基-双-α-萘胺磺酸钠)、亚甲基蓝、二苯乙烯染料(比色指数(CI)=620)、和1,1′-二乙基-2,2′-花青氯化物(CI=374(橙色)或CI=518(蓝色))。这些染料的性质及其制备方
法公开在E.H.Land的“Colloid Chemistryn(1946)中。这些染料在聚乙烯醇中有显著的二向色性,在纤维素中有较小的二向色性。发现刚果红在PEN中稍有二向色性。
这些染料的性质及其制备方法公开在Kirk Othmer Encyclopediaof Chemical Technology,Vol.8,pp.652-661(4th Ed·1993),以及其引用的文献中。
当二向色性染料用于本发明的光学体中时,它可以加入连续相或分散相中。然而,二向色性染料最好能加入分散相中。
二向色性染料与某种聚合物系统结合表现出使光发生不同程度偏振的能力。聚乙烯醇和某些二向色性染料可用来使薄膜有使光偏振的能力。其它聚合物,如聚对苯二甲酸乙二醇酯或聚酰胺,如尼龙-6,在与二向色性染料组合时并没有表现出如此强的使光偏振的能力。因此可以说,聚乙烯醇和二向色性染料的组合比相同染料在其它成膜聚合物系统中的二向色性比要高。较高的二向色性比表明有较高的使光偏振的能力。
二向色性染料在根据本发明制得的光学体中的分子排列最好在将染料加入光学体中后通过拉伸光学体来实现。然而,其它方法也可用来实现分子排列。因此,在一个方法中,二向色性染料(如通过升华或从溶液中结晶出来),在光学体取向前或取向后,结晶入一系列在薄膜或其它光学体表面上用切削、蚀刻或其它方法形成的伸长凹槽中。然后,处理过的表面可用一种或多种表面层涂布、可加入聚合物基质中或用于多层结构中,或可用作另一光学体的组分。凹槽可根据预先确定的方式或图案、以及预定的凹槽间距来制成,以获得所需的光学性质。
在一个相关的例子中,二向色性染料可在将中空纤维或导管放入光学体中之前或之后放大一种或多种中空纤维或其它导管中。中空纤维或导管可用与光学体中的周围材料相同或不同的材料制成。
在还有一个例子中,在将某种层结合入多层结构中之前,将二向色性染料升华到层表面上,从而使其沿多层结构的层界面布置。在还有一个例子中,二向色性染料被用来至少部分回填根据本发明制得的微空隙薄膜中的空隙。本发明的应用
本发明的光学体特别可用作漫射偏振器。然而,光学体也可根据本发明制成反射偏振器或漫射镜。在这些应用中,光学材料的结构与上述漫射应用中的相同。然而,这些反射器在至少一个轴上的折射率差通常很大。此折射率差通常至少约为0.1、更佳的约为0.15、最佳的约为0.2。
反射偏振器在一个轴上存在折射率差,而在另一个轴上则基本匹配。另一方面,反射薄膜在至少两个薄膜平面内的正交轴上的折射率不同。然而,这些例子中的反射性质并不须只靠折射率不匹配来获得。因此,例如,可通过调节薄膜的厚度,来获得所需的反射程度。在一些例子中,调节薄膜厚度可使薄膜由透射漫射器变成漫反射器。本发明的光学体对于电磁辐射的至少一种偏振方向,所述第一和第二相沿至少一个轴一起获得的漫反射率至少约为30%,优选为50%。对于所述的电磁辐射的第一偏振方向,所述光学体的总反射率大于约50%,大于约60%较好,大于约70%更好,对于电磁辐射的正交于所述第一偏振方向的第二偏振方向,所述光学体的总透射率大于约50%,大于约60%较好,大于约70%更好。60%以上的以正交于光束第一光偏振方向偏振的光中,至少有约40%以小于约8°的偏转角透过所述的光学体,至少约有60%较好,至少约有70%更好。
本发明的反射偏振器可以有许多不同的用途,特别可用于液晶显示板。另外,偏振器可用PEN或类似材料(它应是良好的紫外线滤光器,可有效吸收直至可见光谱边界的紫外光)制成。反射偏振器也可用作红外线薄层偏振器。实施例综述
下列实施例描述了本发明的各种光学材料的制备,以及这些材料的光谱性质。除非另有说明,组成百分比指重量组成百分比。用于这些样品的聚萘二甲酸二醇酯树脂是用乙二醇和2,6-萘二甲酸二甲酯(从Amoco Corp.,Chicago,Illinois购得)制成的。这些试剂用传统的聚酯树脂聚合方法来聚合成有不同的特性粘度(IV)的材料。间规聚苯乙烯(sPS)可根据美国专利4,680,353(Ishihara等)公开的方法制得。实施例包括下面讨论的各种聚合物配对、连续相和分散相的各种分数以及其它添加剂或方法变化。用于本发明的连续相和分散相为热塑性树脂聚合物。
样品的拉伸或取向可用常规的用来制备聚酯薄膜的取向设备或实验室分批取向机(laboratory batch orienter)来实现。所用的实验室分批取向机被设计成使用从挤塑流延卷材上切下并被列成方阵的24个夹持器(每侧6个)夹持的小片流延材料(7.5cm×7.5cm)。样品的取向温度用热空气鼓风机来控制,薄膜样品通过一个以控制的速度在一个或两个方向上增加夹持器间距离的机械系统取向。在两个方向上拉伸的样品可以相继地或同时取向。对于以受约束模式(c)取向的样品,所有的夹持器夹住网,且夹持器只在一个方向上移动。而在非约束模式(U)中,在垂直拉伸方向的固定方向上夹住薄膜的夹持器并没有夹住,从而使薄膜可在该方向上松弛或颈缩。
偏振漫透射和反射用装有Perkin Elmer Labsphere S900-1000 150毫米积分球附件和Glan-Thompson立方体偏振器的Pcrkin Elmer Lambda19紫外/可见/近红外分光光度计来测定。平行和正交的透射和反射值分别用电场矢量平行或垂直于薄膜拉伸方向的偏振光来测定。所有扫描是连续的,用480纳米/分钟的扫描速率和2纳米的狭线宽度进行扫描。反射以“V-反射”方式进行。透射和反射值是对400至700纳米范围内所有波长的平均值。实施例I
在实施例1中,用传统挤塑和流延方法将一混合物流延成约380微米厚的薄膜或薄层来制得本发明的光学薄膜,其中混合物有75%聚萘二甲酸乙二醇酯(PEN)作为连续相或主要相,25%聚甲基丙烯酸甲酯(PMMA)作为分散相或次要相。PEN的特性粘度(IV)为0.52(在60%苯酚/40%二氯苯中测定)。PMMA从ICI Americas,Inc.,Wilmington,Delaware获得,产品名为CP82。所用的挤塑机是有单管6Oμm Tegra过滤器的3.15cm(l.24”。)Brabender。模头是30.4cm(l2″)EDIUltraflexTM40。
在薄膜挤塑后约24小时后,流延薄膜在聚酯薄膜拉幅装量上在宽度方向即横向(TD)上取向。拉伸在约9.1米/分钟(30英尺/分钟)下进行,伸长的宽度约为14Ocm(55英寸),拉伸温度约为160℃(320°F)。经拉伸的样品的总反射率用Lambda19分光光度仪上的积分球辅件来测定,样品光束用Glan-Thompson立方体偏振器起偏。样品有75%的平行反射率(即,用电场矢量平行于薄膜拉伸方向的偏振光测得的反射率)和52%正交反射率(即,用电场矢量与拉伸方向垂直的偏振光测得的反射率)。
实施例2
在实施例2中,按实施例1中的方法制备和评价光学薄膜,只是采用的混合物含有75%PEN、25%间规聚苯乙烯(sPS)、0.2%聚苯乙烯甲基丙烯酸缩水甘油酯相容剂和各0.25%的IrganoxTM 101O和UltranoxTM626。聚苯乙烯甲基丙烯酸缩水甘油酯的合成在《塑料、树脂、橡胶、粘合剂和纤维的化学技术(Chemical Technology of Plastics,Resins,Rubbers,Adhensives and Fibers》(Vol.10,chap.3,pp.69-109(1956),Calvin E·Schildknecht编辑)的。“聚合物加工”(Polymer Processes)中有所描述。
PEN在60%苯酚/40%二氯苯中测得的特性粘度为0.52。sPS是从Dow Chemical Co.购得,重均分子量约为200,000(因此以下称为sPS-200-O)测得经拉伸的膜样品的平行反射率为73.3%,正交反射率为35%。
实施例3
在实施例3中,按实施例2的方法制备和评价光学薄膜,只是将相容剂的含量增加到0.6%。测得平行反射率为81%,正交反射率为35.6%。
实施例4
在实施例4中,用传统的三层共挤塑方法制备本发明的三层光学薄膜。薄膜有一个芯层,芯层两侧各有一皮层。芯层是75%PEN和25%sPS 200-4(名称sPS-200-4指含有4%(摩尔)对甲基苯乙烯的间规聚苯乙烯共聚物)的混合物,每一皮层为100%的PEN(在60%苯酚/40%二氯苯中测得的特性粘度为0.56)。
得到的三层流延薄膜中芯层的厚度约为415微米,每一皮层各约为110微米厚,总的厚度约为635微米。在约129℃的温度下,用实验室分批拉伸机(laboratory batch strecher)在纵向(MD)上以约6比1的拉伸比拉伸所得到的三层流延薄膜。由于实验室拉伸机没有夹住薄膜样品平行于拉伸方向的边缘,因此样品在横向(TD)上没有限制,样品由于拉伸而在TD上的颈缩约为50%。
光学性能用实施例1中的方法进行评价,测得平行反射率为80.1%,正交反射率为15%。这些结果表明,薄膜是低吸收、节约能量的体系。
实施例5-29
在实施例5-29中,用实施例4中的方法制备和评价一系列的光学薄膜,只是所用的芯层中的sPS分数和PEN树脂的IV不同(如表1所示)。对于一确定的样品,芯层中PEN树脂的IV与皮层中的相同。流延薄层的总厚度约为625微米,其中总厚度的约三分之二为芯层,其余为厚度大致相等的两个皮层。制备了芯层中的PEN和sPS的不同混合物(如表1所示)。在表1所示的不同温度下,以约6∶1的拉伸比在纵向(MD)或横向(TD)上拉伸薄膜。一些样品在垂直于拉伸方向的方向上受到约束(C),以防止样品在拉伸时颈缩。表1中用“U”标记的样品是未受约束的,它可在非约束方向上颈缩。沿平行和正交(即垂直)于拉伸的方向测定经拉伸的样品的某些光学性质,包括透射、反射和吸收百分比。结果总结在表1中。
实施例24-27中指出的热定形是通过人工约束拉伸样品的两个垂直于拉伸方向的边缘,将其固紧在大小合适的刚性框架上,然后将固紧的样品放入指定温度下的烘箱内1分钟来实现的。样品平行于拉伸方向的两侧没有受到约束(U),即没有固紧,可以颈缩。实施例29中的热定形采用相同的方法,只是拉伸样品的所有四个边缘都是约束(C)的,即固紧的。实施例28没有进行热定形。
表1
实施例编号 | 拉伸温度(℃) | 拉伸方向(MD/TD) | 拉伸约束(C/U) | PEN的IV | 分数(sPS) | 热定形温度 | 受约束的热定形 | 透射率(垂直) | 透射率(平行) | 反射率(垂直) | 反射率(平行) |
5 | 135 | TD | C | 0.53 | 0.25 | 76.2 | 20.4 | 22.6 | 75.3 | ||
6 | 135 | TD | C | 0.47 | 0.75 | 80.2 | 58.4 | 19.4 | 40 | ||
7 | 142 | TD | C | 0.53 | 0.25 | 74.2 | 21.8 | 25.3 | 77.3 | ||
8 | 142 | TD | C | 0.47 | 0.75 | 76.0 | 41.0 | 23.8 | 55.6 | ||
9 | 129 | TD | C | 0.53 | 0.25 | 71.2 | 21.2 | 26.5 | 76.2 | ||
10 | 129 | TD | C | 0.47 | 0.75 | 76.8 | 48.9 | 22.4 | 49.6 | ||
11 | 129 | MD | U | 0.53 | 0.25 | 81.5 | 27.6 | 17.2 | 67 | ||
12 | 129 | TD | U | 0.53 | 0.25 | 66.8 | 22.1 | 25 | 71.9 | ||
13 | 129 | MD | U | 0.47 | 0.25 | 79.5 | 20.3 | 19.3 | 73.7 | ||
14 | 129 | TD | U | 0.47 | 0.25 | 66.3 | 26.2 | 32.5 | 69.4 | ||
15 | 129 | TD | U | 0.47 | 0.5 | 73.0 | 26.2 | 24.7 | 68.7 | ||
16 | 129 | MD | U | 0.47 | 0.5 | 75.4 | 20.6 | 23.2 | 76.1 | ||
17 | 129 | MD | U | 0.47 | 0.1 | 82.1 | 27.3 | 16.9 | 67 | ||
18 | 129 | MD | U | 0.56 | 0.25 | 80.1 | 15.0 | 18 | 80.3 | ||
19 | 129 | TD | U | 0.56 | 0.25 | 70.2 | 21.6 | 25.2 | 70.7 | ||
20 | 129 | MD | C | 0.47 | 0.25 | 75.8 | 28.7 | 23.4 | 70.1 | ||
21 | 129 | MD | C | 0.47 | 0.5 | 79.8 | 27.8 | 19.7 | 70.8 | ||
22 | 135 | MD | C | 0.47 | 0.1 | 80.5 | 36.7 | 19.2 | 62.6 | ||
23 | 135 | MD | C | 0.53 | 0.25 | 77.2 | 21.1 | 21.8 | 76.6 | ||
24 | 129 | MD | U | 0.56 | 0.25 | 150 | U | 83.7 | 17.3 | 17.3 | 74 |
25 | 129 | MD | U | 0.56 | 0.25 | 220 | U | 82.1 | 16 | 18 | 75.8 |
26 | 129 | MD | U | 0.56 | 0.25 | 135 | U | 84.7 | 17 | 18 | 75.3 |
27 | 129 | MD | U | 0.56 | 0.25 | 165 | U | 83 | 16 | 16.5 | 76.3 |
28 | 129 | MD | U | 0.56 | 0.25 | 对照 | 83.7 | 17 | 17.5 | 76 | |
29 | 129 | MD | U | 0.56 | 0.25 | 230 | C | ||||
29 | 129 | MD | U | 0.56 | 0.25 | 230 | C |
对上述所有样品进行观察,发现分散相有各种形状,与分散相在薄膜样品物体中的位置有关。发现较接近样品表面的分散相掺杂物是伸长的形状,而不是更接近球形。较靠近样品两个表面之间中心部分的掺杂物更接近球形。甚至是有皮层的样品也是如此,只是效应被皮层削弱。皮层的加入可减少拉伸操作中破裂的趋势从而改善了薄膜的加工。
不拟与理论结合,认为流延薄膜芯层中掺杂物(分散相)的伸长是混合物通过模头时受剪切的结果。这一伸长特征可通过改变模头的物理尺寸、挤塑温度、挤出物的流动速度、以及连续相和分散相的可改变其相对熔体粘度的化学因素来改变,某些应用受益于分散相在挤塑时的一定伸长。对于那些随后在纵向拉伸的应用,以挤塑时伸长的分散相作为起始,可使得到的分散相有较高的纵横比。
另一值得注意的特点是,当相同样品不受约束地拉伸时,发现性能有显著改善。因此,在实施例13中,透射率在平行和垂直方向上分别为79.5%和20.3%。相反,实施例20中的透射率在平行和垂直方向上分别只有75.8%搜和28.7%。样品在不受约束地拉伸时,与约束拉伸相比,厚度增加,但是由于透射性和消光性改善,因此折射率匹配可能得到了改善。
另一种控制折射率的方法是改变材科的化学性质。例如,30%重量的从对苯二酸获得的共聚单元与70%重量的从2,6-萘二甲酸获得的单元的共聚物的折射率比100%PEN聚合物低0.02个单位。其它单体或比例有稍稍不同的结果。这种变化可用来使一个轴上的折射率匹配得更接近,而只使希望有较大差异的轴上的匹配稍稍降低。换句话说,一个轴上折射率值更接近地匹配所得到的好处足以补偿在希望有较大差别的正交轴上折射率差的降低而有余。第二,可用化学上的变化来改变拉伸发生的温度范围。sPS和各种比例的对甲基苯乙烯单体的共聚物可改变最佳拉伸温度范围。为了最有效地优化整个加工系统以及获得的折射率匹配和差异,可能需要将这些技术结合起来。因此,通过优化与拉伸条件有关的加工和化学因素,并进一步调节材料的化学性质以使至少一个轴上的折射率差尽量增大而至少一个正交轴上的折射率差尽量减小,就可改善对最终性能的控制。
如果这些样品在MD上取向,而不是在TD上取向(对比实施例14-15),那么它们可表现出更好的光学性能。不拟与理论结合,据信采用MD取向而不是TD取向可产生不同几何结构的掺杂物,且这些掺杂物有较高的纵横比,从而使非理想的末端效应变得不重要。非理想的末端效应指在伸长颗粒的每端顶部的几何结构和折射率之间的复杂关系。颗粒的内部或非末端被认为有均一的几何结构和折射率,这是所希望的。因此,均一的伸长颗粒的百分比越高,光学性能就越好。
这些材料的消光比是垂直于拉伸方向的偏振光的透射率与平行于拉伸方向的偏振光的透射率之比。对于表1中列出的实施例来说,消光比在约2至5的范围内,尽管发现根据本发明制得的光学体有高达7的消光比。预计通过调节薄膜厚度、掺杂物体积分数、颗粒大小和折射率匹配和不匹配程度可获得更高的消光比。
实施例30-100
在实施例30-100中,用表2中列举的材料来制备本发明的样品。PEN42、PEN47、PEN53、PEN56和PEN60指在60%苯酚/40%二氯苯中测得的特性粘度(IV)分别为0.42、0.47、0.53、0.56、和0.60的聚萘二甲酸乙二醇酯。所用的特定sPS-200-4是从Dow Chemical Co.购得。EcdelTM 9967和EastarTM是共聚酯,它们是从Eastman chemical Co.,Rochester,New York购得。SurlynTM 1706是离子键树脂,从E.I.du Pontde Nemours & Co.,Wilmington,Delaware购得。列举的作为添加剂1或2的材料包括聚苯乙烯甲基丙烯酸缩水甘油酯。名称GMAPS2、GMAPS5和GMAPS8分别指共聚物总量中有2、5和8%重量的甲基丙烯酸缩水甘油酯。ETPB指交联剂乙基三苯基溴化鏻。PMMA VO44指聚甲基丙烯酸甲酯,从Atohaas North America,Inc.购得。
光学薄膜样品按实施例4的方法制备,除了下表2中所示的不同外。其中列出的主要相是连续相及其与总量的比。次要相是分散相及其与总量之比。报道的混合物厚度的值表示芯层的近似厚度(微米)。皮层厚度随芯层厚度而改变,但是始终保持恒定的比值,即,两个皮层厚度大致相等,两个皮层厚度之和约为总厚度中分散相的大小。那些随后用实验室分批取向机来拉伸的实施例在分批拉伸栏内用“×”表示。
表2
实施例号 | 主要相 | 主要相(%) | 次要相 | 次要相(%) | 芯层(微米) | 添加剂1 | 添加剂2 | SEM值 | TEM(微米) | 分批拉伸 |
30 | PEN.42 | 75 | sPS-200-4 | 25 | 9.8 | - | - | - | - | - |
31 | PEN.42 | 75 | sPS-200-4 | 25 | 16.3 | - | - | 10 | - | - |
32 | PEN.47 | 75 | sPS-200-4 | 25 | 9.8 | - | - | - | - | × |
33 | PEN.47 | 75 | sPS-200-4 | 25 | 16.3 | - | - | 8 | - | × |
34 | PEN.47 | 50 | sPS-200-4 | 50 | 9.8 | - | - | - | - | - |
35 | PEN.47 | 50 | sPS-200-4 | 50 | 16.3 | - | - | 5 | - | × |
36 | PEN47 | 90 | sPS-200-4 | 10 | 9.8 | - | - | - | - | - |
37 | PEN.47 | 90 | sPS-200-4 | 10 | 16.3 | - | - | 3 | - | × |
38 | PEN.53 | 75 | sPS-200-4 | 25 | 9.8 | - | - | - | - | - |
39 | PEN 53 | 75 | sPS-200-4 | 25 | 16.3 | - | - | 7 | - | × |
40 | PEN.56 | 75 | sPS-200-4 | 25 | 9.8 | - | - | - | - | - |
41 | PEN.56 | 75 | sPS-200-4 | 25 | 16.3 | - | - | 6 | - | × |
42 | sPS-200-4 | 75 | PEN.42 | 25 | 9.8 | - | - | - | - | - |
43 | sPS-200-4 | 75 | PEN.42 | 25 | 16.3 | - | - | - | - | - |
44 | sPS-200-4 | 75 | PEN.47 | 25 | 9.8 | - | - | - | - | - |
45 | sPS-200-4 | 75 | PEN.47 | 25 | 16.3 | - | - | - | - | × |
46 | sPS-200-4 | 75 | PEN.53 | 25 | 16.3 | - | - | - | - | - |
47 | sPS-200-4 | 75 | PEN.53 | 25 | 9.8 | - | - | - | - | - |
48 | spS-200-4 | 75 | PEN.56 | 25 | 9.8 | - | - | - | - | - |
49 | sPS-200-4 | 75 | PEN.56 | 25 | 16.3 | - | - | - | - | - |
50 | PET.60 | 75 | EcdelTM9967 | 25 | 16.3 | - | - | - | - | - |
51 | PET.60 | 75 | SurlynTM1706 | 25 | 16.3 | - | - | 2 | - | - |
52 | PEN.47 | 75 | EcdelTM9967 | 25 | 16.3 | - | - | 2 | - | × |
53 | PEN.47 | 100 | - | - | 16.3 | - | - | - | - | - |
54 | PEN.47 | 75 | sPS-200 | 25 | 16.3 | - | - | - | - | - |
55 | PEN.47 | 75 | spS-200 | 25 | 9.8 | - | - | 10 | - | - |
56 | PEN.47 | 75 | sPS-320 | 25 | 9.8 | - | - | 12 | - | - |
57 | PEN.47 | 75 | sPS-320 | 25 | 16.3 | - | - | - | - | - |
58 | PEN.47 | 95 | sPS-320 | 5 | 9.8 | - | - | - | - | - |
59 | PEN.47 | 95 | sPS-320 | 5 | 16.3 | - | - | - | - | - |
60 | PEN.56 | 100 | - | - | 16.39.8 | - | - | - | - | × |
61 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | - | - | 10 | - | - |
62 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | - | - | - | - | × |
63 | PEN.56 | 95 | sPS-200 | 5 | 9.8 | - | - | - | - | - |
64 | PEN.56 | 95 | sPS-200 | 5 | 16.3 | - | - | - | - | × |
65 | PEN.56 | 75 | sPS-320 | 25 | 9.8 | - | - | 10 | - | - |
66 | PEN.56 | 75 | sPS-320 | 25 | 16.3 | - | - | - | - | - |
67 | PEN.47 | 95 | sPS-200 | 5 | 16.3 | 2%GMAPS2 | 0.25%ETPB | 1 | 0.3 | × |
68 | PEN.47 | 95 | sPS-200 | 5 | 9.8 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
69 | PEN 56 | 75 | sPS-200 | 25 | 9.8 | 6%GMAPS2 | 0.25%ETPB | - | - | - |
70 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 6%GMAPS2 | 0.25%ETPB | 0.5 | 2.5 | × |
71 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 2%GMAPS2 | 0.25%ETPB | - | 0.8 | - |
72 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 2%GMAPS2 | 0.25%ETPB | 1 | - | - |
73 | PEN.56 | 95 | sPS-200 | 5 | 9.8 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
74 | PEN.56 | 95 | sPS-200 | 5 | 16.3 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
75 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 6%GMAPS2 | 0.25%ETPB | - | - | - |
76 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 6%GMAPS2 | 0.25%ETPB | 0.8 | 1 | × |
77 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
78 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
79 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 6%GMAPS2 | 0.25%ETPB | - | - | - |
80 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 6%GMAPS2 | 0.25%ETPB | - | - | × |
81 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 6%GMAPS2 | 0.25%ETPB | - | - | - |
82 | PEN.56 | 75 | sPS-200 | 25 | 16.3 | 6%GMAPS2 | 0.25%ETPB | 0.5 | - | - |
83 | PEN.56 | 95 | sPS-200 | 5 | 9.8 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
84 | PEN.56 | 95 | sPS-200 | 5 | 16.3 | 2%GMAPS2 | 0.25%ETPB | - | - | - |
85 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 0.5%GMAPS2 | 0.25%ETPB | - | - | - |
86 | PEN.56 | 75 | sPS-200 | 25 | 9.8 | 0.5%GMAPS2 | 0.25%ETPB | - | - | - |
87 | PEN.47 | 75 | Eastar | 25 | 16.3 | - | - | - | - | × |
88 | PEN.47 | 75 | Eastar | 25 | 9.8 | - | - | - | - | - |
89 | PEN.47 | 75 | Eastar | 25 | 16.3 | - | - | - | - | - |
90 | PEN.47 | 75 | Eastar | 25 | 9.8 | - | - | - | - | - |
91 | PEN.47 | 75 | PMMAVO44 | 25 | 9.8 | - | - | - | - | - |
92 | PEN.47 | 75 | PMMAVO44 | 25 | 16.3 | - | - | 10 | - | - |
93 | PEN.47 | 75 | PMMAVO44 | 25 | 16.3 | 6%MMA/GMA | - | - | 0.7 | - |
94 | PEN.47 | 75 | PMMAVO44 | 25 | 9.8 | 6%MMA/GMA | - | - | - | - |
95 | PEN.47 | 75 | PMMAVPO44 | 25 | 9.8 | 2%MMA/GMA | - | - | 1.2 | - |
96 | PEN.47 | 75 | PMMA | 25 | 16.3 | 2%MMA/GMA | - | - | - | × |
97 | PEN.47 | 75 | sPS-200-4VO44 | 25 | 916.3 | 0.5%刚果红 | - | - | - | × |
98 | PEN.47 | 75 | sPS-200-4 | 25 | 16.3 | 0.15%刚果红 | - | - | - | × |
99 | PEN.47 | 75 | sPS-200-4 | 25 | 9.8 | 0.25%亚甲基蓝 | - | - | - | - |
100 | PEN.47 | 75 | sPS-200-4 | 25 | 9.8 | 0-0.25%亚甲基蓝 | - | - | - | - |
发现各种相容剂的存在可降低掺杂物或分散相的大小。实施例101
在实施例101中,用与实施例4相同的方法制备光学薄膜,只是芯层厚度约为420微米,每层皮层厚度约为105微米。PEN的IV为0.56。流延薄膜如实施例1那样取向,只是拉伸温度为165℃,流延和拉伸间隔15天。平行和垂直与偏振光的透射率分别为87.1%和39.7%。
实施例102-121
在实施例102-121中,光学薄膜如实施例101那样制备,只是取向条件不同和/或如表3所示用含有4或8%(摩尔)对甲基苯乙烯的sPS共聚物,或无规立构的苯乙烯,Styron 663(从Dow Chemical Company,Midland,Michigan购得)代替sPS-200-4。表3中也报道了透射性质的评价结果。透射率值是在450-700nm范围内所有波长的平均值。
表3
实施例 | %sPS | PS | PEN的IV | 拉伸温度(℃) | 滑轨设定值(cm) | 垂直透射率(%) | 平行透射率(%) |
101 | 25 | 200-0 | 0.56 | 165 | 152 | 87.1 | 39.7 |
102 | 35 | 200-0 | 0.56 | 165 | 152 | 87.8 | 44.4 |
103 | 15 | 200-4 | 0.56 | 165 | 152 | 86.1 | 43.5 |
104 | 25 | 200-4 | 0.56 | 165 | 152 | 86.5 | 43.6 |
105 | 35 | 200-4 | 0.56 | 165 | 152 | 88.2 | 50.7 |
106 | 15 | 200-8 | 0.56 | 165 | 152 | 89.3 | 40.7 |
107 | 25 | 200-8 | 0.56 | 165 | 152 | 88.5 | 42.8 |
108 | 35 | 200-8 | 0.56 | 165 | 152 | 88.6 | 43.3 |
109 | 15 | Styron 663 | 0.56 | 165 | 152 | 89.3 | 45.7 |
110 | 25 | Styron 663 | 0.56 | 165 | 152 | 87.8 | 41.6 |
111 | 35 | Styron 663 | 0.56 | 165 | 152 | 88.8 | 48.2 |
112 | 15 | Styron 663 | 0.48 | 165 | 152 | 88.5 | 62.8 |
113 | 25 | Styron 663 | 0.48 | 165 | 152 | 87.1 | 59.6 |
114 | 35 | Styron 663 | 0.48 | 165 | 152 | 86.8 | 59.6 |
115 | 15 | 200-0 | 0.48 | 165 | 152 | 88.0 | 58.3 |
116 | 25 | 200-0 | 0.48 | 165 | 152 | 88.0 | 58.7 |
117 | 35 | 200-0 | 0.48 | 165 | 152 | 88.5 | 60.6 |
118 | 15 | 200-4 | 0.48 | 165 | 152 | 89.0 | 57.4 |
119 | 35 | 200-4 | 0.48 | 165 | 152 | 87.3 | 64.0 |
120 | 35 | 200-0 | 0.56 | 171 | 127 | 86.5 | 65.1 |
121 | 35 | 200-0 | 0.56 | 171 | 152 | 88.1 | 61.5 |
这些实施例表明,在IV高的PEN中,掺杂相颗粒在纵向上的伸长比在低IV的PEN中要多。这与在低IV的PEN中发现发生在靠近薄膜表面处的伸长比发生在薄膜内部的要多是一致的,其结果是在靠近表面处形成纤维状结构,在接近中央处形成球形结构。
这些实施例中的一些表明,取向温度和取向程度是实现所需效果时的重要变量。实施例109至114表明,静止结晶并不一定是的优选的偏振光缺乏透射的唯一原因。
实施例122-124
在实施例122中,用209层供料头(feedblock)制备本发明的多层光学薄膜。供料头用两种材料进料:(1)以38.6kg/小时的速率输入的PEN(特性粘度为0.48);和(2)95%CoPEN和5%(重量)sPS均聚物(分子量为200000)的混合物。CoPEN是基于70%(摩尔)萘二甲酸酯和30%(摩尔)间苯二酸二甲酯的共聚物,与乙二醇聚合至特性粘度为0.59。CoPEN/sPS混合物以34.1千克/小时的速率加入至供料头中。
CoPEN混合材料是在挤出物的外侧,得到的叠层的薄层组分在两种材料间交替变化。薄层厚度设计成制得四分之一波长叠层中的各层厚度具有线性梯度,最薄层与最厚层的比例为1.3。然后将较厚的不含sPS的CoPEN皮层(根据上述制备CoPEN/sPS混合物的方法制备,只是摩尔比是70/15/15萘二甲酸酯/对苯二酸二甲酯/间苯二酸二甲酯)施加到209层复合体的每一侧。总的皮层以29.5干克/小时的速度施加,叠层每一侧或表面上约有此量的一半。
将得到的有皮层覆盖的多层复合体挤塑通过一个倍增器(multiplier),以得到421层的多层复合体。然后,得到的多层复合体用另一70/15/15 CoPEN皮层以29.5千克/小时的总速度在每一表面上包覆,每一侧上约为此量的一半。由于这第二皮层并不能从存在的皮层上分别测得(因为材料是相同的),为了这里的讨论,得到的非常厚的皮层将按一层来计算。
得到的421层复合体再一次挤塑通过比例为1.40的不对称扩增器,以获得841层的薄膜,然后薄膜挤塑通过一模头并骤冷浇铸成约30密耳厚的片。然后,得到的浇铸薄片用传统的制膜拉幅装置来在宽度方向上取向。薄片在约300°F(149℃)下拉伸,拉伸比约为6∶1,拉伸速度约为20%/秒。得到的经拉伸的薄膜约5密耳厚。
在实施例123中,按实施例122的方法制备多层光学薄膜,只是CoPEN/sPS混合物中sPS的量为20,而不是5。
在实施例124中,按实施例122的方法制备多层光学薄膜,只是薄膜中不加入sPS。
表4中的结果包括了薄膜的光增益测定结果。薄膜的光增益是薄膜放在背光源与LCD面板之间时由背光源发出而透射通过面板的光与没有薄膜时透射的光之比。关于光学薄膜意义光增益的意义在WO95/17692中参照该文献附图2有所描述。通常希望有较高的增益值。透射值包括当光源在平行于拉伸方向(T‖)偏振和垂直于拉伸方向(T⊥)时得到的数值。偏离角色彩(OAC)是用Oriel分光光度仪测定波长在400至700nm的50°入射光的p-偏振透射的均方根偏差(root mean squaredeviation)来获得。
表4
实施例 | sPS%(摩尔) | 光增益 | T⊥(%) | T‖(%) | OAC(%) |
122 | 5 | 1.5 | 83 | 2 | 1.5 |
123 | 20 | 1.45 | 81 | 1.5 | 1.2 |
124 | 0 | 1.6 | 87 | 5 | 3.5 |
偏离角色彩(OAC)的数值证明了使用本发明多层结构的优点。特别是,这种结构可用来大大降低OAC,而光增益只适量减少。这一折衰在某些应用中是有利的。本发明实施例的T‖数值比预计的要低,因为sPS分散相散射的光不会被检测器接收。
本发明的以上描述只是说明性的,而没有限制性,因此,应当理解本发明的范围只参照所附权利要求来限定。
Claims (30)
1.一种光学体,包含:
双折射至少为0.05的第一聚合物相;和
分散在所述第一相中的第二聚合物相,其折射率不同于所述第一相,沿一个第一轴方向第一和第二相折射率之差大于0.05,而沿正交于所述第一轴的第二轴方向上所述折射率之差小于0.05,其特征在于:对于电磁辐射的至少一种偏振方向,所述第一和第二相沿至少一个轴一起获得的漫反射率至少为30%。
2.如权利要求1所述的光学体,其特征在于:所述第一相的双折射至少为0.1。
3.如权利要求1或2所述的光学体,其特征在于:所述第二相的双折射小于0.02。
4.如权利要求1或2所述的光学体,其特征在于:所述第二相的折射率不同于所述第一相的折射率,沿所述第一轴方向,所述折射率之差大于0.1。
5.如权利要求1或2所述的光学体,其特征在于:所述的第二相的折射率不同于所述第一相,沿所述第二轴方向,所述折射率之差小于0.03。
6.如权利要求1或2所述的光学体,其特征在于:对于电磁辐射的两个偏振方向,所述第一和第二相沿所述至少一个轴一起获得的漫反射率至少为50%。
7.如权利要求1所述的光学体,其特征在于:对于所述的电磁辐射的第一偏振方向,所述光学体的总反射率大于50%;对于电磁辐射的正交于所述第一偏振方向的第二偏振方向,所述光学体的总透射率大于50%。
8.如权利要求7所述的光学体,其特征在于:至少有40%的以正交于光束的第一偏振方向偏振的光以小于8°的偏转角透过所述的光学体。
9.如权利要求1或2所述的光学体,其特征在于:所述的第一相包含一种热塑性树脂。
10.如权利要求9所述的光学体,其特征在于:所述的热塑性树脂是由乙烯基芳香单体衍生的间规立构乙烯基芳香聚合物。
11.如权利要求9所述的光学体,其特征在于:所述的热塑性树脂包括间规立构的聚苯乙烯的共聚单元。
12.如权利要求9所述的光学体,其特征在于:所述的热塑性树脂包括聚萘二甲酸乙二醇酯。
13.如权利要求12所述的光学体,其特征在于:所述的第二相包括间规立构的聚苯乙烯。
14.如权利要求9所述的光学体,其特征在于:所述的第二相还包括至少一种热塑性聚合物。
15.如权利要求1所述的光学体,其特征在于:对所述的光学体进行拉伸,拉伸比至少为2至6。
16.如权利要求1或2所述的光学体,其特征在于:至少在两个方向上使所述光学体定向。
17.如权利要求1或2所述的光学体,其特征在于:存在的所述第二相相对所述第一相的体积分数为15%至30%。
18.如权利要求1或2所述的光学体,其特征在于:对于可见光、紫外或红外电磁辐射的至少一个偏振方向,所述第一和第二相沿至少一个轴向一起获得的漫反射率至少为30%。
19.如权利要求1或2所述的光学体,其特征在于:所述光学体是薄膜;沿垂直所述薄膜表面的第三轴,所述第一相与第二相之间的折射率差小于0.05,所述第三轴与所述第一和第二轴相互正交。
20.如权利要求1或2所述的光学体,其特征在于:至少在一个方向上对所述光学体进行拉伸;至少有40%的正交于光束的第一偏振方向的偏振光漫射透过所述光学体;所述的漫透射光线主要分布在圆锥表面上或其附近,圆锥表面包含镜面透射方向而圆锥轴以拉伸方向为中心。
21.如权利要求1或2所述的光学体,其中所述的光学体为偏振薄膜。
22.如权利要求1或2所述的光学体,其还含有一种二向色性染料。
23.如权利要求22所述的光学体,其特征在于:所述的二向色性染料分散在所述第二相中。
24.如权利要求1或2所述的光学体,
其特征在于:沿所述第一轴所述第一与第二相的折射率之差的绝对值为Δn1,而沿正交于所述第一轴的第二轴为Δn2,这里,Δn1与Δn2之差的绝对值至少为0.05。
25.如权利要求24所述的光学体,其特征在于:Δn1与Δn2之差的绝对值至少为0.1。
26.如权利要求24所述的光学体,其特征在于:所述第一相的双折射大于所述第二相的双折射。
27.如权利要求26所述的光学体,其特征在于:所述第一相的双折射比所述第二相的双折射至少大0.02。
28.如权利要求25所述的光学体,其特征在于:所述第二相沿任何三个相互垂直轴中的至少两个轴是不连续的。
29.如权利要求28所述的光学体,其特征在于:该光学体是一种偏振片。
30.如权利要求29所述的光学体,其特征在于进一步包含二向色性染料。
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US08/610,092 US5825543A (en) | 1996-02-29 | 1996-02-29 | Diffusely reflecting polarizing element including a first birefringent phase and a second phase |
US08/610,092 | 1996-02-29 |
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CN97194162A Pending CN1217068A (zh) | 1996-02-29 | 1997-02-28 | 含光学膜的灯具 |
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CN97194162A Pending CN1217068A (zh) | 1996-02-29 | 1997-02-28 | 含光学膜的灯具 |
CN97192655A Pending CN1212764A (zh) | 1996-02-29 | 1997-02-28 | 具有光引出器的光导纤维 |
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