CN1295524C - 具有附加层的多层聚合物薄膜 - Google Patents
具有附加层的多层聚合物薄膜 Download PDFInfo
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- CN1295524C CN1295524C CNB028082958A CN02808295A CN1295524C CN 1295524 C CN1295524 C CN 1295524C CN B028082958 A CNB028082958 A CN B028082958A CN 02808295 A CN02808295 A CN 02808295A CN 1295524 C CN1295524 C CN 1295524C
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Abstract
一种含有由很多交替的聚合物层组成的光学推栈的多层聚合物薄膜,该堆栈的表层具有与堆栈中的层不同的机械、光学或化学性质。在一个实施方案中,该多层聚合物薄膜含有一个或多个全息图,能够产生吸引人而有用的光学效果。
Description
发明背景
众所周知,多层光学堆栈能提供许多种光学性质。这样的多层光学堆栈可用作反射偏振器或反射镜,反射各种偏振的光。它们也可用作具有波长选择性的反射器,例如只反射可见光,而让红外线透过的“冷镜”;或者是让可见光透过,而反射红外线的“热镜”。美国专利5882774中有许多各种已有光学堆栈的例子。
本领域已知的多层光学堆栈的问题,是这些光学堆栈本身可能不具备所有需要的物理、化学和光学性质。因此需要某种其他方法来提供这些所需的性质。
发明简述
根据本发明的一个实施方案,至少有一层附加层附着在多层膜的一个或两个主表面上,该附加层具有与光学堆栈中的层不同的机械、化学或光学性质。
根据本发明的另一实施方案,至少有一层附加层附着在多层膜的一个或两个主表面上,该附加层起保护多层光学堆栈的作用。
根据本发明的又一实施方案,对某些结构,包括全息的图象(也称为“全息图”),和多层光学堆栈将进行描述。
附图简述
图1A,1B和2为优选的多层光学膜。
图3到图8是实施例1到实施例6的多层光学膜的光透射率谱图。
图9为本发明的多层膜,有一附加层粘附与其一个主表面上。
图10为根据本发明制造的一个多层膜,该膜的两个主表面都附着有附加层。
图11为一个多层膜,该膜的一个主表面附着有一层附加层,而另一个表面附着有两层附加层。
图12到图18为本发明的各种实施方案,都包括一个多层膜和一个全息图。
图19到到图20描述了本发明含有全息图的实施方案,与偏振器使用。
优选实施方案详述
多层光学膜
上述的美国专利5882774对多层光学膜的优点、特征和制造进行了很全面的描述。多层光学膜,例如用作高效的镜子和(或)偏振器。下面将对多层光学膜的性质和特征进行相对简要的叙述,然后对使用本发明多层光学膜的说明性背光系统实施方案将进行叙述。
本发明所使用的多层光学膜对入射光的吸收较低,对斜射的和正射的光线有很高的反射能力。这些性质都成立,不管这些膜是用于光的纯粹反射还是反射偏振。多层光学膜具有这些独特的性质和优点,这就使其可用来设计高效背光系统,相对于已有的背光系统,该背光系统具有较低的吸收损失。
图1A和1B为本发明的典型的一个多层光学膜,它包括一个光学堆栈10,光学堆栈由至少两种材料12和14的层交替组成。至少一种材料具有应力产生双折射的性质,因此拉伸过程就会影响该材料的折射率(n)。图1A为拉伸前的一个典型的多层光学堆栈,其中两种材料有相同的折射率。光线13经历极小的折射率改变,通过光学堆栈在图1B中,该光学堆栈经过了拉伸,材料12的折射率变大。层间折射率的不同导致部分光线15被反射。通过对多层光学堆栈从单轴方向一直到双轴方向的拉伸,就制造了对不同方向的平面偏振入射光具有一个范围不同反射率的膜。这样,这个多层光学堆栈就可用做反射偏振器或反射镜。
根据本发明制造的多层光学膜具有一个布鲁斯特角(当光入射在任何层间界面时反射系数趋近为0时的角),对于聚合物层界面而言,布鲁斯特角很大或者根本就不存在。与此不同,已知的多层聚合物膜在层间界面显示相对较小的布鲁斯特角,这导致光的透射和(或)不希望发生的彩虹效应。然而,根据本发明制造的多层光学膜能使其p偏振光的反射率随着入射角增大而缓慢降低的镜子和偏振镜的结构和入射角没有关系,或者随着入射角增大而增大。因此,多层光学堆栈对于s和p偏振光在很宽的波长范围内,在很宽的入射角范围内都具有很高的反射率。
图2为多层光学堆栈的两层,标出了每层的三维折射率。n1x,n1y和n1z指102层的折射率,n2x、n2y和n2z指104层的折射率。各层的折射率之间的关系以及层间折射率的关系就决定了多层光学堆栈在任何入射角,偏离任何方位的反射特性。在美国专利5882774中所叙述的原理和设计时需考虑的事项都可用来制造在各种环境和用途中具有所需光学效果的多层光学堆栈。操控和改变多层光学堆栈中各层的折射率,可以得到需要的光学性质。
再次看看图1B,多层光学堆栈10可以包含数十、数百或数千层,每层都可由很多不同材料中的任意一种制成。某个特定光学堆栈的所需性能决定了所选材料必须具备什么特征。光学堆栈所用的材料的种类数目可以多至和层数一样。但是,为制造方便,优选的光学薄膜光学堆栈仅含有少许几种不同的材料。
不同材料或化学性质相同但物理性质不同的材料之间的界面可能是突然的或逐步的。除了在一些简单情况下有分析方法外,对后者这种分层的并且有连续变化的折射率的情况进行分析时,一般将其分成很多均匀的薄层,层间有明显的界面,但相邻层性质的变化很小。
优选的多层光学堆栈由一对对低/高折射率层组成,每对低/高折射率层的联合光学厚度是它设计要反射的光的波段的中心波长的1/2。这样的光学堆栈一般被称为1/4波长光学堆栈.对于要反射可见光和近红外线的多层光学膜而言,四分之一波长光学堆栈的设计使得该光学堆栈的每层的平均厚度不超过0.5微米。
在需要用到反射膜(如镜子)的用途中,各偏振方向和各入射平面的光所需的平均透射率一般决定于该反射膜的预期作用。双轴拉伸多层光学堆栈是制造多层反射膜的一种方法。对于一个高效反射膜,可见光(380~750nm)垂直入射时在不同拉伸方向的平均透射率希望低于10%(反射超过90%),优选为低于5%(反射超过95%),更优选为低于2%(反射超过98%),尤其选为低于1%(反射超过99%)。波长为380~750nm的光以偏离法线60度的入射角入射时,其平均透射率希望是低于20%(反射超过80%),优选为低于10%(反射超过90%),尤其优选为低于5%(反射超过95%),更优选为低于2%(反射超过98%),更优选为低于1%(反射超过99%)。
此外,不对称的反射膜可能有某些特定的用途。在此情况下,一定波长范围内的光,例如可见光(380~750nm)或可见光连同近红外光(380-850nm),在某个拉伸方向上的透射率希望是低于例如50%,而在其他拉伸方向上的平均透射率希望是低于例如20%。
多层光学膜也可用作反射偏振器,单轴拉伸多层光学堆栈是制造多层反射偏振器的一种方法。所制造的反射偏振器对于偏振面与其轴(拉伸方向)平行的光在很宽的入射角范围内都有高的反射率;而对于偏振平面与另一轴(未拉伸方向)平行的光在很宽的入射角范围内都有低的反射率和高的透射率。通过控制各个膜三个折射率nx、ny和nz,就能得到希望的偏振器性能。
在很多的应用中,理想的反射偏振器在所有的入射角范围内,在一个轴(称为消光轴)上有高反射率,而在另一个轴(称为透射轴)上有零反射。对于偏振器的透射轴,一般都希望当所选的波长范围的光以所选入射角范围入射时,在透射轴方向偏振的光的透射能达到最大。
当可见光(380~750nm,300nm带宽)垂直入射偏振器时,在透射轴上的平均透射率希望至少是50%,优选为至少70%,更优选为至少80%,尤其优选为至少90%。可见光(380~750nm)以偏离法线60度的入射角入射偏振器时,平均透射率(沿透射轴测量p-偏振光而得)希望至少是50%,优选至少为70%,更优选至少为80%,尤其优选至少为90%。
可见光波长范围内(380~750nm,300nm带宽)在消光轴方向偏振所得的光垂直入射多层反射偏振器时,其平均透射率希望是低于50%,优选为低于30%,更优选低于15%,尤其优选低于5%。波长范围在380~750nm范围内在消光轴方向偏振所得的光以偏离法线60度的入射角入射到偏振器时,其平均透射率(沿透射轴测量p-偏振光而得)希望低于50%,优选为低于30%,更优选低于15%,尤其优选低于5%。
在某些应用中,当偏振平面平行透射轴的p-偏振光斜射时优选具有高反射率。沿透射轴偏振的光以至少偏离法线20度的入射角入射时,其平均反射率应超过20%。
此外,虽然在这里是分开讨论反射偏振膜和不对称反射膜的,但应该理解,当使用两个或更多的这样的膜时,可以基本上反射照射到它们上的光(只要适当地调整这些膜相互的取向)。当多层光学膜被用作在根据本发明的背光系统中的反射器时,就一般需要上述的结构。
如果在透射轴方向发生部分反射,当光线斜射时偏振器的效率会降低。如果在透射轴方向的放反射率随波长而改变,透射的光将会有不同的颜色。求出所选波长范围的光以选择的角度入射时的透射率的均方根(RMS值),这是衡量颜色的一种方法。RMS颜色百分数根据以下公式确定:
其中,积分范围λ1和λ2是所选的波长范围即带宽,
T是沿透射轴的透射率,T是在所选波长范围内沿透射轴的平均透射率。对于希望得到较低颜色的偏振器的场合,当光以偏离法线至少30度,优选为偏离法线至少45度,更优选为偏离法线至少60度的入射角入射时,RMS颜色百分数应该低于10%,优选为低于8%,更优选为低于3.5%,尤其优选为低于2%。
反射偏振器在所选的带宽内,优选地同时在透射轴方向上具有所需的RMS颜色百分数(有特定的用途)和在消光轴方向有所需的反射率。当可见光波长范围内(400~700nm,带宽300nm)的光垂直入射到偏振器上时,沿消光轴方向的平均透射率希望是低于40%,更希望是低于25%,优选为低于15%,更优选为低于5%,尤其优选为低于3%。
材料的选择和工艺过程
根据上文提到的美国专利5882774中所述设计中需考虑的方面,普通技术人员会认识到,很多种材料都可用来制造本发明的多层反射膜或偏振器,只要在制造过程中选择条件以获得所需的折射率关系。可以通过很多种方法获得所需的折射率关系,包括在膜成形过程中或之后拉伸膜(例如是有机聚合物时),挤压(例如是液晶材料时),或涂覆。此外,最好是两种材料具有相似的流变学性质(例如熔体粘度),这样就可以同时挤压。
一般而言,合适的材料组合是选用结晶或半结晶材料,或液晶材料,最好是聚合物中作为第一种材料。第二种材料则可以是结晶、半结晶或无定形材料。第二种材料可以具有与第一种材料相反或相同的双折射。或者第二种材料没有双折射。应该认识到,在聚合物领域人们广泛认为聚合物是典型的非完全结晶的材料,因此在本发明的表述中,结晶或半结晶聚合物是指那些不是无定形的,包括那些一般称为结晶、部分结晶或半结晶等的材料。第二种材料可能具有与第一种材料相反或相同的双折射。第二种材料也可以没有双折射。
适用材料的具体例子有聚萘二甲酸乙二醇酯(PEN)和其同分异构体(例如2,6-,1,4-,1,5-,2,7-和2,3-PEN),聚对苯二甲酸亚烷基二酯(例如聚对苯二甲酸乙二酯,聚对苯二甲酸丁二酯,聚对苯二甲酸-1,4-二亚甲基环己酯),聚酰亚胺(例如聚丙烯酰亚胺),聚醚酰亚胺,不规则聚苯乙烯,聚碳酸酯,聚甲基丙烯酸酯(例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(例如聚丙烯酸丁酯和聚丙烯酸甲酯),间规聚苯乙烯(sPS)、间规聚-α-甲基苯乙烯,间规聚二氯苯乙烯,共聚物和任何这些聚苯乙烯的混合物,纤维素衍生物(例如乙基纤维素,醋酸纤维素,丙酸纤维素,醋酸-丁酸纤维素和硝酸纤维素),聚烯类聚合物(例如聚乙烯,聚丙烯,聚丁烯,聚异丁烯和聚4-甲基戊烯),含氟聚合物(例如全氟烷氧树脂,聚四氟乙烯,氟化乙烯-丙烯共聚物,聚偏二氟乙烯和聚氯三氟乙烯),含氯聚合物(例如聚偏二氯乙烯和聚氯乙烯),聚砜,聚醚砜,聚丙烯腈,聚酰胺,有机硅树脂,环氧树脂,聚醋酸乙烯酯,聚醚胺,离子键树脂,弹性体材料(例如聚丁二烯,聚异戊二烯,氯丁(二烯)橡胶),聚氨酯。共聚物也适合,例如PEN的共聚物(coPEN),例如2,6-,1,4-,1,5-,2,7-和/或2,3-萘二酸或酯与(a)对苯二甲酸或酯,(b)异酞酸或酯,(c)邻苯二甲酸或酯,(d)二元醇,(e)环二元醇(例如环己二甲醇),(f)直链二元羧酸,(g)环二元羧酸(例如环己二羧酸)形成的共聚物;聚对苯二甲酯乙二醇酯共聚物,例如对苯二甲酸或酯与(a)萘二甲酸或酯,(b)异酞酸或酯,(c)邻苯二甲酸或酯,(d)二元醇,(e)环二元醇(例如环己二甲醇),(f)直链二元羧酸,(g)环二元羧酸(例如环己二羧酸)形成的共聚物;聚苯乙烯的共聚物,例如苯乙烯-丁二烯共聚物和苯乙烯-丙烯腈共聚物;4,4’-二苯甲酸和乙二醇共聚物。此外,每层都可能包括两种或两种以上上述的聚合物或共聚物(例如间规聚苯乙烯(sPS)和无规苯乙烯的混合物)。上述的coPEN也可能是球粒的混合物,其中至少一种组分是以萘二甲酸为基础的聚合物,其他组分是其他聚酯或聚碳酸酯,比如PET,PEN或coPEN。
偏振器各层的优选组分包括PEN/coPEN,聚对苯二甲酸乙二醇(PET)/coPEN,PEN/sPS,PET/sPS,PEN/Estar和PET/Estar,其中“coPEN”指以萘二甲酸(如上所述)为基础的共聚物或混合物,Estar是指可从Eastman化学药品公司购买的聚对苯二甲酸二亚甲基环己酯。
反射膜各层的优选组合包括PET/Ecdel,PEN/Ecdel,PEN/sPS,PEN/THV,PEN/co-PET和PET/sPS,其中co-PET指以对苯二甲酸(如上所述)为基础的共聚物或混合物,Ecdel指可从Eastman化学药品公司购买的一种热塑性聚酯,THV是可从明尼苏达州St.Paul的明尼苏达矿业与制造公司购得的含氟聚合物。
由于膜厚度、柔性和经济性方面的原因,应采用尽可能少的层数以达到希望的光学性质。偏振器和反射膜的层数优选为少于10000层,更优选少于5000层,尤其优选少于2000层。
如上所述,制造多层膜工艺过程中的条件将会影响到产品达到满意的各折射率之间的关系(也就是多层膜的光学性质)的能力。对于可通过拉伸取向的有机聚合物,一般通过共挤压聚合物得到多层膜,然后在选择的温度下拉伸该膜,之后可在某温度下对该膜热定形,从而制得所需膜。挤压和取向步骤也可以同时进行。在一个方向(单轴取向)上对膜充分拉伸来制造偏振器,在两个方向(双轴取向)上充分拉伸来制造反射膜。
可以让膜从横向拉伸方向上的自然的收缩(等于拉伸比的平方根)状态在横向拉伸方向上进行尺寸松弛;对这种松弛可以加以限制,以便减小横向拉伸方向上大的尺寸变化;或者可主动地在横向拉伸方向上进行拉伸。可以例如使用长度取向器(length orienter)将膜进行纵向拉伸,或者使用拉幅机对膜进行宽度方向的拉伸。
通过选择拉伸前的温度、拉伸温度、拉伸速率、拉伸比、热定形温度、热定形时间、热定形松弛率和横向拉伸松弛率,可以制得具有满意折射率关系的多层膜。这些变量是相互依赖的,例如,举个例子,如果拉伸温度相对较低,就可以使用相对较低的拉伸速率。普通的技术人员可以知道如何选择合适的变量组合,来制得满意的多层膜。然而,一般希望在拉伸方向上的拉伸比为1∶2到1∶10(优选为1∶3到1∶7),在横向于拉伸方向上的拉伸比为1∶0.2到1∶10(优选为1∶0.2到1∶7)。
制造合适多层膜的方法,还有适用于双折射聚酰亚胺的旋涂法(例如在文献Boese等,J.Polym.Sci.:Part B,30:1321(1992)所述)和适用于结晶有机化合物的真空沉积法(例如在文献Zang等,Appl.Phys.Letters,59:823(1991)所述);后种技术对结晶有机化合物和无机材料的某些组合特别有用。
在以下实施中将叙述一些典型的多层反射镜和多层反射偏振器。
实施例1
(PEN:THV500,449,镜)
先在在一次操作中将浇注带材进行挤压,然后用一台实验室薄膜拉伸机对所得的膜进行拉伸取向,从而制得含有449层的共挤出复合薄膜。一台挤压机以56磅/小时的速度对本征粘度为0.53dl/g(在60重量%苯酚和40重量%二氯苯的溶液中测量)的聚对萘二甲酸乙二醇酯(PEN)进行挤压,另一台挤压机以11磅/小时的速度对THV500(可从明尼苏达矿业与制造公司购得)进行挤压。PEN位于表层,同时50%的PEN在两个表层中。使用供料头方法制得57层,然后通过三个倍增装置得到含有449层的挤出物。作为挤压原料的浇注带材的厚度为20密耳,宽度为30.4厘米。然后使用一台实验室拉伸机对薄膜进行双轴取向,该拉伸机用一个动臂装置紧夹薄膜的一个正方形部分,同时匀速地向两个方向拉伸薄膜。在100℃将边长为7.46的方形薄膜装到拉伸机上,在60秒内升温到140℃。然后,以10%/s(相对于原尺寸)的速率开始拉伸,直到样品被拉伸到3.5×3.5。样品拉伸结束以后,立即用室温空气吹上去进行冷却。
图3为此多层膜的透射率。曲线(a)为在透射方向偏振的光垂直入射时的透射率,曲线(b)为在透射方向偏振的p-偏振光以60度入射时的透射率。
实施例2
(PEN:PMMA,601,镜)
通过共挤压工艺,在一条连续平展膜生产线上制得含有601层的共挤出复合膜。挤压机A以114磅/小时的速度对本征粘度为0.57dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN)进行挤压,其中64磅/小时的PEN到供料头,剩下的进入列表层中,如下面所述。挤压机B以61磅/小时的速度对PMMA(英国化学工业公司北美分公司提供的CP-82)进行挤压,所有的料都到供料头。PEN在供料头的一些表层中。供料头方法制得151层,此时使用象在美国专利3801429中叙述的供料头,在此供料头之后用挤压机C以30磅/小时的速度对PEN(与挤压机a挤压PEN是同一类型)共挤压制得两对称的表层。该挤出物经过两个倍增器得到含有601层的挤出物。在美国专利3565985中也叙述了类似的共挤压倍增器。该挤出物经过另一台装置,该装置以总共50磅/小时的速度将从挤压机A出来的PEN共挤压形成表层。制得的膜在138℃进行纵向拉伸取向,拉伸比约为3.2。然后预热,在38秒内加热到154℃,之后以11%/小时的速度横向拉伸,拉伸比为4.5。然后,在227℃下无松弛地进行热定形。最终膜的厚度为3密耳左右。
由图4的曲线(a)可见,350nm带宽的光垂直入射时,整个波长范围内的平均消光率大于99%。光吸收的数值很小,因此难以测量,但应该低于1%。当以偏离法线50度入射时,s-偏振光(曲线(b))和p-偏振光(曲线(c))消光程度相近,和预料的一样,波段都向短波长方向移动。由于s-偏振光的较大带宽和在PEN层中p-偏振光的较低折射率,s-偏振光的红波段边缘向蓝波段边缘的移动没有p-偏振光那么强烈。
实施例3
(PEN:PCTG,449,偏振器)
先在在一次操作中将浇注带材挤压,然后用一台实验室薄膜拉伸机对所得膜进行拉伸取向,制得含有449层的复合薄膜。此时采用供料头方法,其中使用了61层供料头和三个(2x)倍增器。在最后倍增器和模头之间,将厚的一些表层加了上去。一台挤压机以25.0磅/小时的速度将本征粘度为0.47dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN)供给到供料头。另一台挤压机以25.0磅/小时的速度供给二醇改性对苯二甲酸二亚甲基环己酯(PCTG5445,Eastman)。从上述挤压机出来的另一股PEN在倍增器之后以25.0磅/小时的速度作为表层加了上去。所用的浇注带材厚0.18mm,宽30.5cm。然后使用一台实验室拉伸机对薄膜进行单轴拉伸取向,该拉伸机用一个动臂装置紧夹薄膜的一部分,匀速地向一个方向拉伸薄膜,在其他方向允许其自由松弛。装上的膜样品的宽为5.40cm左右(在未被固定的方向),在动臂装置的两个夹子之间长度为7.45cm。100℃下,将膜装到拉伸机上,然后在45秒内升温到135℃。然后以20%/小时(相对与原来的尺寸)的速度开始拉伸,直到膜被拉伸到6∶1(以夹子之间的距离进行测算)。拉伸之后,立即用室温空气吹样品冷却之。样品中部的松弛因数子为2.0。
图5为此多层膜的透射率曲线,其中曲线(a)为在非拉伸方向上偏振的光垂直入射时的透射率,曲线(b)为在非拉伸方向上偏振的p-偏振光以60度入射时的透射率,曲线(c)为在拉伸方向上偏振的光垂直入射时的透射率。曲线(a)在400~700nm波段的平均透射率为89.7%,曲线(b)在400~700nm波段的平均透射率为96.9%,曲线(c)在400~700nm波段的平均透射率为4%。曲线(a)的RMS颜色百分数为1.05%,曲线(b)的RMS颜色百分数为1.44%。
实施例4
(PEN:coPEN,601,偏振器)
通过共挤压工艺,在一条连续平展膜生产线上制得含有601层的共挤出复合膜。一台挤压机以75磅/小时的速度对本征粘度为0.54dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN)挤压,另一台挤压机以65磅/小时的速度对coPEN挤压。coPEN是由70摩尔%的2,6-萘二甲酸甲酯,15摩尔%的异酞酸二甲酯和15摩尔%的乙二醇改性对苯二甲酸甲酯。采用供料头方法制得151层。供料头设计为生成一叠从上到下厚度逐渐变化的膜,最厚的膜与最薄的膜的厚度比为1.22。在该光学堆栈外面采用共挤压制得一些PEN表层,其总厚度为共挤出膜的8%。光学堆栈经过两个连续的倍增器倍增之。两个倍增器的额定倍增比分别为1.2和1.27。随后,膜在40秒内被预热到154℃,然后以6%/s的速率横向拉伸,拉伸比约为5.0。最后得到的膜的厚度约为2密耳。
图6为此多层膜的透射率曲线。曲线(a)为在非拉伸方向上偏振的光垂直入射时的透射率,曲线(b)为在p-偏振光以60度入射时的透射率,曲线(c)为在拉伸方向上偏振的光垂直入射时的透射率。应当注意当p-偏振光垂直入射和以60度入射时,在非拉伸方向上的透射率都很高(80~100%)。也应当注意曲线(c)显示的在拉伸方向上偏振的,可见光波段(400~700nm)的光具有很高的反射率。在500nm到650nm之间的反射率几乎达到100%。
实施例5
(PEN:sPS,481,偏振器)
481层的多层薄膜由从Eastman化学试剂公司购买的本征粘度为0.56dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN)和间规均聚聚苯乙烯(sPS,重均分子量为200000道尔顿,从Dow公司购买)制备。PEN在外层,其挤压速度为26磅/小时,sPS的挤压速度为23磅/小时。使用供料头方法制造了61层,每层的厚度相近。供料头之后使用三个倍增器(2x)。在最后倍增器之后,加上了具有相同厚度的两个表层,它含有与进入供料头相同的PEN,供料速度为22磅/小时。浇注带材通过宽为30.5cm的模头挤压,得到厚度为0.276mm的膜。挤压温度为290℃。
在环境条件下保存制得的膜9天,然后用用拉幅机进行单轴伸取向。薄膜先在25秒内被预热到160℃,然后以25%/秒的速率横向拉伸,最后的拉伸比为6∶1。在拉伸方向不允许松弛。成品薄膜的厚度约为0.046mm。
图7为该含有481层的PEN:sPS反射偏振器的光学性能图。曲线a为在非拉伸方向上偏振的光垂直入射时的透射率,曲线b为p-偏振光以60度入射时的透射率,曲线c为在拉伸方向上偏振的光垂直入射时的透射率。应当注意当p-偏振光垂直入射和以60度入射时有高透射率。曲线a中400~700nm范围的平均透射率为86.2%,曲线b中400~700nm范围的平均透射率为79.7%。也应注意曲线c显示的在拉伸方向上偏振的可见光波段(400~700nm)的光具有很高的反射率。曲线c在400~700nm范围的平均透射率为1.6%。曲线(a)的RMS颜色百分数为3.2%,而曲线(b)的RMS颜色百分数为18.2%。
实施例6
(PEN:coPEN,603,偏振器)
通过共挤压工艺,在一条连续平展膜生产线上制得含有603层的反射偏振器。一台挤压机以83磅(38kg)/小时的速度挤压本征粘度为0.47dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN),另一台挤压机以75磅(34kg)/小时的速度挤压coPEN。coPEN是由70摩尔%的2,6-萘二甲酸甲酯,15摩尔%的异酞酸二甲酯和15摩尔%的乙二醇改性对苯二甲酸甲酯组成。采用供料头方法制得151层。供料头设计为生成一叠从上到下厚度逐渐变化的膜,最厚的膜与最薄的膜的厚度比为1.22。光学堆栈经过两个连续的倍增器倍增之。两个倍增器的额定倍增数分别为1.2和1.4。在最后倍增器和模头之间,用第三台挤压机以106磅(46kg)/小时的速度供料,将表层复合上,该表层由与上述相同的coPEN组成。然后在30秒内将该薄膜预热到150℃,之后以20%/秒的初速率横向拉伸该膜,拉伸比约为6。成品膜的厚度约为0.089mm。
图8为实施例6的偏振器的光学性能。曲线a为在非拉伸方向上偏振的光垂直入射时的透射率,曲线b为p-偏振光以50度入射时的透射率,曲线c为在拉伸方向上偏振的光垂直入射时的透射率。应当注意在非拉伸方向上偏振的光的具有很高的透射率。曲线a中400~700nm范围的平均透射率为87%。也应注意曲线c显示的在拉伸方向上偏振的可见光波段(400~700nm)的光具有很高的反射率。曲线c在400~700nm范围的平均透射率为2.5%。此外,该偏振器的RMS颜色百分数非常低。曲线(b)的RMS颜色百分数为5%。
虽然如上所述的多层光学堆栈具有有意义的和满意的光学性质,但其本身却很难提供其他的性质,可能是机械的,光学的或化学的性质,而如果不具备这些性质,将降低光学堆栈的性能。可以在光学堆栈上再复合一层或多层,这些层能提供光学堆栈的上述性质,但并不提供光学堆栈本身的光学功能。这些层一般是复合在主表面上的,因此一般被称为表层。
表层可在制造多层膜的过程中被共挤压到光学堆栈的一个或两个主表面上,以保护多层光学堆栈不受在供料头和模壁上的高剪切力破坏;可在组成表层的聚合物中加入添加剂,如UV稳定剂,使得表层得到需要的化学或物理性质,然后在多层光学堆栈的制造过程中在多层光学堆栈的一面或两面将具有改变性质的表层共挤压上去。在多层膜的制造过程中也可将附加层共挤压到表层的外面上;附加层也可以以单独的操作覆盖上去;或以分离的膜、箔、刚性的或半刚性的增强层、如聚酯(PET)、聚丙烯酸酯(PMMA)、聚碳酸酯、金属或玻璃的形式叠压到多层膜上。用来将多层聚合物膜叠压到另一表面的胶粘剂包括光学透明的和半透明的胶粘剂,还包括压敏和非压敏的胶粘剂上。压敏胶粘剂一般在室温下就具有粘性,至多用手指轻微地压一下就能将其粘到表面上,而非压敏胶粘剂有溶剂、热和辐射致粘系统。本发明中用到的一些胶粘剂例子,其主要成份为聚丙烯酸酯;聚乙烯醚;含二烯橡胶例如天然橡胶、聚异戊二烯和聚异丁烯;聚氯戊二烯;丁基橡胶;丁二烯-丙烯腈共聚物;热塑性弹性体材料;嵌段共聚物例如苯乙烯-异戊二烯和苯乙烯-异戊二烯-苯乙烯嵌段共聚物、乙烯-丙烯-二烯共聚物和苯乙烯-丁二烯共聚物;聚α烯烃;无定形聚烯烃;硅树脂;含乙烯的共聚物例如乙烯-乙酸乙烯酯共聚物、乙烯丙烯酸酯共聚物、甲基丙烯酸乙酯共聚物;聚氨酯;聚酰胺;环氧树脂;聚乙烯吡咯烷酮和乙烯基吡咯烷酮聚合物;聚酯;以及上述物质的混合物。此外,胶粘剂中可含有添加剂,例如增粘剂,增塑剂,填料,抗氧化剂,稳定剂,颜料,漫射性颗粒,固化剂,生物杀灭剂和溶剂。本发明中优选的胶粘剂为VITEL3300——可从Shell化学公司购买的一种热熔胶粘剂或得自Minnesota Mining and Manufacturing Co.的丙烯酸类压敏胶粘剂如90/10 IOA/AA丙烯酸类胶粘剂。当使用胶粘剂将多层薄膜粘附到另一表面上时,要对胶粘剂的组成和厚度进行选择,以便不影响多层光学堆栈的光学性质。例如,要在希望具有高透射率的多层聚合物偏振器或镜上覆盖附加层时,所用的胶粘剂应当在偏振器或镜子设计要透射的波长范围内保持光学透明。
图10和11分别为含有1层和2层附加层的多层光学堆栈的示意图。在下面叙述可应用的各种附加层时,将用到图10和11。
单轴取向的多层光学堆栈,例如反射偏振器特别需要具有不同机械性质的表层。这样的光学堆栈一般在主拉伸方向上具有低的抗撕裂性。这将导致在制造过程中的产率降低或在后续使用中的破损。为防止这些,可在光学堆栈的外主表面上粘附抗撕裂层。这些结实的层可由任何合适的材料组成,甚至可由光学堆栈中的一种材料组成。选择抗撕裂层材料时需考虑的因素有破坏伸长率、杨氏模量、抗撕裂强度、与内层的粘合力在所选电磁波长范围内的透射率和吸收率、光学透明度或浑浊度、折射率与光频率而变化的的关系、质地和粗糙度、熔融热稳定性、分子量分布、熔融态流变学性质和共挤压性能、所附加的韧层和光学层材料的混溶性和互扩散速率、拉伸条件下的粘弹性、松弛和结晶行为、在使用温度的热稳定性,耐候性、粘合于涂层的能力和对各种气体和溶剂的渗透性。当然,如上所述,重要的是所选择的材料不能具有对光学堆栈光学性能有害的光学性质。附加层可在制造过程中施加到光学堆栈上去,也可以后再叠压到光学堆栈上。在制造过程中将这些附加层粘合到光学堆栈上,例如通过共挤压,其好处是在光学堆栈制造过程中能保护光学堆栈。
用图10来说明本发明的这一方面,图10为具有抗撕裂层的多层光学堆栈示意图。薄膜400包括光学堆栈410,光学堆栈410包括交替的层412和414,这两种层分别由具有不同光学性质的聚合物组成。附在光学堆栈410主表面上的是抗撕裂层416和418。需要说明的是,虽然图10中层416和418比412和414厚,但对一般首选的实施方案中尺寸是不合比例的。一般而言,希望层416和418每层的厚度要比光学堆栈的厚度的5%大。层416和418每层的厚度优选为光学堆栈厚度的5%到60%之间,这样既能提供抗撕裂性,又能不增加不必要的材料使用量。这样,如果光学堆栈有600层,在这样的优选实施例中抗撕裂层416和418每层的厚度将与光学堆栈30到360层的厚度相等。在一更好的实施方案中,抗撕裂层416和418每层的厚度在光学堆栈厚度的30%到50%之间。
在一特别好的实施方案中,抗撕裂外层可以是由交替层412和414所用的材料中的一种形成。具体是,已发现在由交替PEN层和coPEN组成的反射偏振器中,可在其制造过程中共挤压得到coPEN的抗撕裂外层。
实施例7
由交替的PEN和coPEN形成的多层薄膜制成的反射偏振器,与厚的coPEN表层共挤压形成抗撕裂反射偏振器。在连续平展膜挤压机上制得含有603层的共挤出复合膜。
一台挤压机以86磅/小时的速度挤压本征粘度为0.47dl/g(在60重量%的苯酚和40重量%的二氯苯的溶液中测量)的聚对萘二甲酸乙二酯(PEN),另一台挤压机以78磅/小时的速度挤压coPEN。coPEN是由70摩尔%的2,6-萘二甲酸甲酯和30摩尔%的乙二醇改性对苯二甲酸甲酯组成。采用供料头方法制得151层。供料头被设计为生成一叠从上到下厚度逐渐变化的膜,最厚的膜与最薄的膜的厚度比为1.22。光学堆栈经过两个连续的倍增器倍增之。两个倍增器的额定倍增数分别为1.2和1.27。在最后倍增器和模头之间,含有上述coPEN的层加上去。用第三台挤压机装料和出料这些层,总共的速度为187磅/小时。然后在40秒内将具有附加coPEN外层的薄膜预热到160℃,之后以20%/秒的初速率横向拉伸,拉伸比约为6。成品膜的厚度约为100μm,其中内部的多层光学堆栈的厚度约为50μm,两层外部层(薄膜的两边各一层)的厚度分别为25μm左右。该膜的抗撕裂性得到了提高,如果没有表层,即使是很坚固的的反射偏振器也会受到损坏。具体是,根据ASTMD-1938方法,在主拉伸方向上采用“裤子撕裂测试”测定了本发明所制造有coPEN表层的膜和在相同条件下制造但没有coPEN表层的膜的抗撕裂性。薄膜的平均厚度分别为100μm和48μm,平均撕裂力分别为60.2克力和2.9克力,其标准偏差分别为4.44和0.57克力。对coPEN表层的分析显示低的取向,在633nm波长的折射率为1.63、1.62和1.61。很难完全把层分开,这就证实了具有很好的层间粘结性。为进行进一步的比较,还测试了具有3.8μm外部PEN层的48μm厚的光学堆栈,其平均撕裂力为2.8克,标准偏差为1.07。
通过附加一层含有可吸收一个或多个选择波长范围的光的颜料或染料的表层,可改变薄膜的外观和性能,波长范围包括部分或全部的可见光,还有紫外和红外。当然,如果所有的可见光都被吸收,这个层就是不透明的。为了改变透射膜的光或被薄膜反射的光的颜色,可以进行选择。这些膜也可含有具有荧光性质的颜料或染料。选择荧光材料是为了在紫外区域吸收电磁波能量,再放射出可见光。它们也可用来修饰膜的性质,尤其是在薄膜能让一些频率的光透射而反射另外频率的光时。例如,图9就是这样一个薄膜的示意图,层316是含有电磁波吸收材料的层。
在覆盖层中使用UV吸收或保护材料尤为可取,因为它可用来保护那些当曝露在UV辐射下可能不稳定的内层。较好的保护材料包括阻胺光稳定剂(HALS),该稳定剂可应用于图9中的层316或图10中的层416和层418的一层或两层中,美国专利No.5605761详细地叙述了该稳定剂。
在另一类较好材料中的压敏胶粘剂可应用于图9中的层316或图10中的层416和层418的一层或两层中。当打算将光学堆栈以后叠压到另一种材料如玻璃或金属基材上时,一般可使用压敏胶粘剂。
另一种可应用于表层如层316或层416和层418的一层或两层的材料是增滑剂。增滑剂可使得薄膜在制造过程中更易处理。增滑剂一般用于镜膜,而不使用于让一部分入射光透射的薄膜。含有增滑剂的一面通常是在准备叠合到支持基材的那一面,这样是为了防止增滑剂由于反射而增加薄膜的浑浊度。
另一种可使用的附加层是保护层。这样的层可以是抗磨损或抗风蚀和/或抗化学腐蚀的。当多层膜将暴露于严酷的或腐蚀性的环境时,这样的涂层尤其有用。抗磨损或坚硬的外层的例子有丙烯酸类树脂坚硬涂层,例如可从Rohm&Haas购买的Acryloid A-11和Paraloid K-120N;丙烯酸氨基甲酸酰胺,例如在美国专利No.4249011中所述的,可从Sartomer公司购买;例如由聚异氰酸脂族酯(例如可从Miles Ins.购买的Desmodur N-3300)和聚酯(例如可以Union Carbide购买的Tone Polyol 0305)反应制得的聚氨酯。这些层同样也可防止气体例如氧气、二氧化碳或水蒸气通过薄膜。同样,这种层可以是图9所示的单层或图10所示的两面有的层。
图11为含有交替层512和514,保护层516、518和520的交替多层薄膜。因此,在多层光学堆栈的一个主表面上可存在不止一层的附加层。在具有图11所示结构的例子中,层516和518为上述的抗撕裂层,层520为抗磨损层。
其他可附加的层包括含有全息图,全息漫射体的层或其他漫射层。这些层可在硬的聚合物或胶粘剂中。预成形的全息材料,例如全息热冲压箔或全息层合薄膜,可附加到多层膜的外表面上。全息材料要么含有金属化不透明效果的铝反射器,要么含有具有基本透明效果的高折射率反射器。通过加热和施加压力,全息热冲压箔可附加到多层膜的表面。型号为VC55-101G的一种典型的透明全息热冲压箔和型号为BD68-100F的一种典型的不透明全息热冲压箔现在可从Crown Roll Leaf of Paterson,New Jersy购得。全息薄膜可通过热熔或压敏胶粘剂中的任一种附加到多层膜上。型号为XLT-101W的一种典型的透明全息薄膜现在可从Crown Roll Leaf购得。型号为9458的一种典型压敏胶粘剂现在可从Minnesota Mining and Manufacturing Company,St.Paul,Minnesota(3M)购得。在多层膜的表面上或透过多层膜可以看到全息图象。
对此领域的技术人员,“全息图象”这个术语可包括全息结构、衍射光栅、电子束形成的结构、激光干涉形成的结构、全息光学元件和光敏聚合物立体全息图。
将这些全息图加入到多层光学薄膜上的方法有两种,一种是直接将全息结构压花到薄膜的外层上;另一种是先涂上一层可压花的树脂,然后再将全息压花在树脂上。此外,在具有全息结构的表面上再附上一层高折射率材料,可提高其可见度和耐久性。此外,还可在上述的高折射率材料上再附上一层保护层或胶粘剂,以便于该薄膜就能附加到物件上去,或者保护其免受指印和擦痕对膜的损害。全息图加入到多层光学薄膜的一种可用的方法,是先在多层光学膜上涂覆一层合适的光敏聚合物,然后将立体全息图记录到光敏聚合物涂层上。
通常全息结构上都有一层附加的反射层,而偏振器、镜和变色镜膜自身的反射使得没有必要再附加这一层。因此,本发明的另一方面是提供一种经济的方法,将全息结构直接压花到多层光学膜上,然后直接在薄膜上涂覆上附加层以增强全息图象。图12到17图示了且实施例8到17都叙述了本发明这些方面的各种实施方案。为了方便,在图12到18中光学堆栈(由第一种聚合物和第二种聚合物形成的交替层)中的交替层只有很少的几层。如这里所述,可以使用许多层。
图12图示了一个含有交替聚合物层602和604以及聚合物表层606和608的多层光学薄膜600。产生全息图象的全息结构610位于表层中。在图13所示的实施方案中,全息结构610上还有一层高折射率层612,层612可用任何适宜的方法加上去,包括真空沉积法。在图14所示的实施方案中,高折射率层612上可有一层保护层614,该保护层可保护全息结构免受损害、污染和其他可降低全息图象质量的环境影响。
图15显示含有一层树脂层616(优选为涂覆方法,但也可以用叠合或其他方法)的多层光学薄膜实施方案,全息结构610就压花在树脂层中。图16所示的实施方案中,树脂层618先浇注在多层薄膜上,然后固化(浇注和固化法),全息结构610就位于浇注和固化的层中。
图17中,全息层620由含有全息结构的树脂层622、高析射率反射层624和胶粘剂层626组成,胶粘剂层626用来将全息层620和多层膜的其余部分粘合在一起。胶粘剂层626可以是压敏胶粘剂、热熔胶粘剂或其他合适的胶粘剂。
图18图示了全息偏振标签630,具有如图12所示的多层膜,和标签本体632通过例如胶粘剂层631将其粘合于标签本体632,该本体包括标签基础膜634,印上的图象636(例如字母与数字构成的或图形的)和用来将标签粘附到基材上的胶粘剂层638。标签或其他这种类型的层合物可以粘贴到有价值的物品上,例如软件、盒子、有价值的文件、护照、生活消费品,例如电子产品和电脑,和其他类似的物品。图19和20显示图18所示的全息偏振标签的使用。当观察者通过在一定取向上保持的鉴定偏振器640看标签时,由全息结构所产生的全息图象和印上的图象636都能看得见。当鉴定偏振器640相对于标签旋转后(鉴定偏振器和标签交叉),印上的图象消失,而全息图象仍能看得见。这样,用户就可鉴定偏振标签的真实性,相应地也就鉴定了贴有标签的物品的真实性。在下面实施例9中还将对此进行进一步描述。
实施例8
由coPEN/PEN交替层制得的偏振器薄膜(从Minnesota Mining andManufacturing Company,St.Paul,Minnesota(3M)购得,其名为“双重亮度提高薄膜”,#98-0440-0037-4)具有半银反射镜的外观。使用下述的方法在薄膜的coPEN外层压花上全息结构,得到如图12所示的薄膜。在全息图模板上电铸上一块镍压花板,制造一公司标志的全息结构,这是在全息图压花工业中常见的。这块板被粘附到一台压花机的圆筒上,这样的机械现在可从James RiverHolographics of Richmond,Virginia购得。带有此压花板的圆筒被加热到93℃。一卷偏振薄膜安装到压花圆筒和被加热到49℃的金属支撑圆筒之间。对这两个圆筒加压使偏振薄膜与压花板接触,结果全息结构就压花到偏振薄膜表面上。这样一卷偏振薄膜就连续而经济地被压花出了全息结构。
由于薄膜的反射镜外观,从薄膜前方观察,能很清楚地看到压花在偏振膜前表面上的公司标志全息结构。当把薄膜反转过来时,从薄膜的后面观察,全息公司标志不是很看得见,这是由于偏振膜反射了一半从薄膜前方入射的光。
实施例9
用胶粘剂将实施例8中制得的已全息压花的偏振膜与印有图象的白色标签的背面粘合在一起,使全息图象露在外面,一般如图18所示。透射半银偏振膜可以看到印在标签上的图象。
为检验全息图象的真实性,称之为检偏器的另一块偏振膜(无全息图象)被放到观察者和具有全息图象的偏振标签之间。当检偏器一直旋转到与含有全息图象的偏振膜交叉时,由于两个交叉的偏振膜的高反射率,位于底部的标签上所印的图象就几乎看不见,而全息图象是可以观察到的,如图20所示。当检偏器旋转90度后,检偏器与具有全息图象的偏振膜平行,位于底部的标签所印的图象又可以看到,而只能模糊地看到全息图象,如图19所示。因此,就可以用检偏器来检验全息图象的真实性。此外,借助能发出至少在两个垂直方向上偏振的光的光源可观察偏振标签的全息图象,也有相同的检验效果。
实施例10
由601层交替的coPEN/PEN聚合物层组成的颜色转换偏振器,其波长上限是590nm,当增大观察角度时,从橙色变到黄色。采用实施例8所述的方法在薄膜的coPEN表层压花上全息图象。然后,如实施例9一样,将薄膜和印有图象的白色标签粘合在一起,全息图象朝前。
用检偏器来检验标签的真实性,当光垂直入射时,颜色从白色变到深橙色,此时检偏器旋转至与具有全息图像的偏振膜交叉。这种独特的,可用检偏器观察到的颜色变化增加了标签的安全性。
实施例11
实施例8的全息偏振膜,其具有全息结构的表面在有些操作条件下很容易被刮坏。此外,来自手印的油会填充全息结构,降低全息图象的可见性。手指油和通常聚合物的折射率与表层的coPEN相近(约为1.6),这样它们与薄膜的折射率相差很小,会导致全息图象的模糊。为避免那些影响,将具有不同折射率的材料用来保护全息结构,一般如图13所示。具有2.34折射率的硫化锌薄膜通过真空沉积法附加到实施例8连续生产出来的偏振膜的全息结构上。
此全息图象的可见度比得上实施例8。由于高折射率层保护了全息结构层,手指油并没有显著地降低全息图象的可见度。美国专利No.4856857(Takeuchi etal.)中其他的这种高折射率层也有这样的用途。
实施例12
在实施例11的全息偏振膜的高折射率层上涂覆上一层附加的保护聚合物层,它具有图14所示的一般结构。用苯胺印刷术将折射率为1.5的UV固化丙烯酸类树脂清漆(名为UV固化苯胺印刷清漆,UVF02037,现在可从Akzo NobelInks Crop,.Langhorne,PA购得)浇注固化上去。
清漆有效地保护了全息结构免受刮伤。由于在实施例12中硫化锌的折射率(2.34)与清漆(1.5)的差别小于在实施例11中硫化锌的折射率(2.34)与空气(1.0)的差别,本实施例中的全息图象的可见度稍微低于实施例11。然而,当使用实施例9中的检偏器进行观察时,实施例12中全息图象的可见度还是可以接受的。
实施例13
本实施例的颜色转换镜膜(名为CM590 Radiant Light Film,#70-4000-0049-6,从3M公司购得)是由224层交替的PET/coPMMA聚合物层组成,并具有反射镜的外观;随着观察角度的增大,变色镜膜从蓝绿色变为蓝色,然后变为紫红色。本薄膜是依据标题为“Color Shifting Film”的PCT Publication WO99/36258叙述的方法制造的。此色的特征在于,颜色的变化与观察角度有关。PET外层不象实施例8偏振膜的coPEN外层一样,能承受压花全息图象过程中的热和压力。因此,首先将透明的PMMA树脂溶液涂在颜色转换膜的前表面,待其干燥。然后,借助一装饰性衍射光栅,采用实施例8的工艺将全息图象压花到膜上,得到图15所示的结构。
从膜的前表面观察,衍射光栅全息图具有很高的可见度,并因膜的折射率而提高。当观察角度增大时,膜的颜色从蓝绿色变为蓝色,然后变为紫红色,这使得全息图象具有一种独特的效果。这种效果可被用来检验全息图象的真实性。
实施例14
在由交替的PEN和PMMA组成的可见光镜膜(名称:VM2000 Radiant MirrorFilm,#70-4000-0069-4,可从3M公司购买)上涂覆10%w/vPMMA(名称:Elvacite2041,可从Dupont,of Wilmington,Delaware购买)甲苯溶液。湿厚度为175微米,95℃下过夜干燥后,在镜膜上得到厚为17-20微米的PMMA膜。使用一块有25美分硬币图象的镍压花片,保持115℃和70吨压力30秒。相对于铝蒸气涂层的反射率95%,本实施例的多层聚合物薄膜具有更高的反射率(>99%),因此全息图象非常明亮。
实施例15
实施例13所述的这种颜色转换薄膜,用硫化锌涂覆,以此来保护薄膜的结构,所用涂覆方法在实施例11中已有描述。如同实施例13,全息图像仍然高度可见。如同实施例12,可以在薄膜上涂上一层丙烯酸类清漆,用来保护薄膜,以免刮伤。另外,具有高折射率的反射镜如美国专利No.4856857(Takeuchi et al.)所述,也可用于此种结构。
实施例16
颜色转换薄膜用PEN/PMMA聚合物如交替224层做成,其波长下限为740纳米。当观察角度逐渐增大时,这种薄膜可以从透明变化到蓝绿色(通常叫做透明到有色的膜),题为“透明变到有色的安全薄膜”的美国专利中也说到这一点,为了提供另外的代表性No.6045894(Jonza et al.)薄膜,一种透明的PMMA树脂可以涂在薄膜的前表面(如实施例13),或者直接将PMMA作为外层来制作薄膜。使用实施例8中的过程,在薄膜上可以进行全息压花。
这种全息图象在薄膜的前表面是可见的。当通过薄膜观察,而结构面对薄膜背面时,图象是可见的。当薄膜的观察角度逐渐增大,颜色从透明变到蓝绿色时,可以检验全息图象的真实性。实施例11中描述的硫化锌及其他高折射率的涂层可以加到这种结构中去。然后可将实施例12中讲到的保护漆或者胶粘剂加到这种结构的上面,所得的全息颜色转换薄膜可以作为层压板使用。
实施例17
为了制造其他代表性结构,可以将全息结构以全息艺术所知的在美国专利No.5948199(McGrew)中所述的方式直接浇注并固化在上述铸造加工在多层光学薄膜的表面上。这种一般类型的结构已在图16中作了说明。如同就压花全息图所述过的,可以附加上高折射率层,保护层及胶粘剂层。
这种多层的光学薄膜,特别是那些全息图象薄膜,有多种用途。可以作为标签,聚合物货币,重要文档(比如护照,标题文档,证书及其他)部件,卡片(比如身份证,驾驶证,信用卡及其他)的部件及消费品(比如玩具,其他产品的包装物或者商店里的其他消费品)的部件。
Claims (10)
1.多层光学薄膜,所述光学薄膜包括:
(a)光学堆栈,所述光学堆栈包括至少第一种聚合物层与第二种聚合物的交替层,并具有第一与第二外层;
(b)压花到至少一个所述外层中的全息图象;
(c)至少一个在全息图象上的附加层。
2.如权利要求1所述的多层光学薄膜,其特征在于,所述至少一个在全息图象上的附加层是高折射率材料。
3.如权利要求2所述的多层光学薄膜,其特征在于,所述薄膜包括在该高折射率材料上的胶粘剂层。
4.如权利要求1所述的多层光学薄膜,其特征在于,所述至少一个在全息图象上的附加层是保护层。
5.权利要求1所述的多层光学薄膜,其特征在于,所述薄膜是一种偏振器。
6.提供这种光学薄膜的方法,所述方法包括如下步骤:
(a)提供包括至少第一种聚合物与第二种聚合物的交替层,并具有第一与第二外层的光学堆栈;
(b)提供压花到至少一个所述外层中的全息图象;
(c)在全息图象上提供至少一层附加层。
7.下列(a)和(b)的组合:
(a)多层偏振器薄膜,含有交替的至少第一种聚合物层和第二种聚合物层以及压花到该多层偏振器薄膜的至少一个外层中的全息图象,该多层偏振器薄膜位于印上的图象的上面;
(b)检验偏振器薄膜;当这两个偏振器薄膜处在至少一个取向时,印上的图象是几乎不能被察觉的,而全息图象则可看到。
8.多层光学薄膜,所述薄膜包括:
(a)光学堆栈,所述光学堆栈包括至少第一种聚合物和第二种聚合物的交替层,其中,至少一种聚合物具有应力引起的双折射功能;
(b)压花到所述光学堆栈的至少一个外层中的通过所述光学堆栈可见的全息图象。
9.权利要求8所述的多层光学薄膜,其特征在于,所述光线含有平均厚度不超过0.5微米的半结晶聚合物层和平均厚度不超过0.5微米的第二种聚合物层,所述光学堆栈至少在一方向上拉伸到至少是未拉伸时的两倍尺寸;所述光学堆栈有第一和第二主表面,每个所述层在其一个平面上有折射率nx和ny,在垂直该平面的方向上有折射率nz,选择所有这些折射率可以达到需要的光学性质。
10.一种多层薄膜,它包括光学堆栈,该光学堆栈包含下述(i)和(ii)的交替层:(i)含有其平均厚度不超过0.5微米的半结晶聚合物层,和(ii)其平均厚度不超过0.5微米的第二种聚合物层,所述光学堆栈至少在一方向上拉伸到至少是未拉伸时的两倍尺寸;所述光学堆栈有第一和第二主表面,每个所述层在所述层的x-y平面有折射率nx和ny,在垂直所述层的x-y平面的方向上有折射率nz,选择所有这些折射率可以达到需要的光学性质;所述薄膜还包括压花在所述光学堆栈的所述第一主表面上的全息图象。
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Also Published As
Publication number | Publication date |
---|---|
ATE362120T1 (de) | 2007-06-15 |
JP2005509179A (ja) | 2005-04-07 |
WO2002084343A1 (en) | 2002-10-24 |
US20020015836A1 (en) | 2002-02-07 |
US6737154B2 (en) | 2004-05-18 |
DE60220040D1 (de) | 2007-06-21 |
EP1379900A1 (en) | 2004-01-14 |
DE60220040T2 (de) | 2008-01-24 |
CN1503916A (zh) | 2004-06-09 |
AR036996A1 (es) | 2004-10-20 |
EP1379900B1 (en) | 2007-05-09 |
JP4279555B2 (ja) | 2009-06-17 |
TWI257349B (en) | 2006-07-01 |
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