CN1153909A - 耐热的起偏振镜 - Google Patents
耐热的起偏振镜 Download PDFInfo
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- CN1153909A CN1153909A CN96101300A CN96101300A CN1153909A CN 1153909 A CN1153909 A CN 1153909A CN 96101300 A CN96101300 A CN 96101300A CN 96101300 A CN96101300 A CN 96101300A CN 1153909 A CN1153909 A CN 1153909A
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- polyvinyl alcohol
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 26
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- 229920001197 polyacetylene Polymers 0.000 claims description 17
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 13
- 238000007789 sealing Methods 0.000 claims description 13
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 9
- 229910000077 silane Inorganic materials 0.000 claims description 9
- 238000005496 tempering Methods 0.000 claims description 8
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- 125000002534 ethynyl group Chemical group [H]C#C* 0.000 claims description 5
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- 229910052736 halogen Inorganic materials 0.000 claims description 2
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- 229920000642 polymer Polymers 0.000 abstract description 6
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- 229910052760 oxygen Inorganic materials 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
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- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910052786 argon Inorganic materials 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000004327 boric acid Substances 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- LIKFHECYJZWXFJ-UHFFFAOYSA-N dimethyldichlorosilane Chemical compound C[Si](C)(Cl)Cl LIKFHECYJZWXFJ-UHFFFAOYSA-N 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
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- 238000007127 saponification reaction Methods 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
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- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
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- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- 239000003377 acid catalyst Substances 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 125000005619 boric acid group Chemical group 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
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- YCEQUKAYVABWTE-UHFFFAOYSA-N dichloro-methyl-prop-2-enylsilane Chemical compound C[Si](Cl)(Cl)CC=C YCEQUKAYVABWTE-UHFFFAOYSA-N 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- MEGHWIAOTJPCHQ-UHFFFAOYSA-N ethenyl butanoate Chemical compound CCCC(=O)OC=C MEGHWIAOTJPCHQ-UHFFFAOYSA-N 0.000 description 1
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
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- 239000001923 methylcellulose Substances 0.000 description 1
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 1
- 150000001282 organosilanes Chemical class 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
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- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
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- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/06—Coating with compositions not containing macromolecular substances
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/02—Physical, chemical or physicochemical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/046—Forming abrasion-resistant coatings; Forming surface-hardening coatings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2349/00—Characterised by the use of homopolymers or copolymers of compounds having one or more carbon-to-carbon triple bonds; Derivatives of such polymers
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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
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
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- Y10T428/264—Up to 3 mils
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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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- Y10T428/31652—Of asbestos
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Abstract
本发明涉及包括具有共轭双键的聚合物起偏振层的耐热的挠性起偏振镜,其表面用Siox(其中x是1-2)保护层密封。
Description
本发明涉及包括具有共轭双键的聚合物起偏振层和SiOx密封表面的耐热的挠性起偏振镜。本发明还涉及与附加的外层粘合的这类起偏振镜。
US 4,818,624描述了用有机硅烷表面甲硅烷基化的方法对光起偏振镜的稳定化。这种方法是不适当的,因为在49-74℃(120-165°F)24时后便可见到褪色和颜色漂移。
从各种底材制造具有粘合中间层的层压制品是已知的。US 5,049,427描述了具有含聚乙炔(PAC)聚合物(POLPAC)的起偏振芯层和透明外层的层压起偏振镜,其中各层是用特定的聚氨酯聚脲粘合在一起的。
尽管POLPAC起偏振镜已经具有极佳的性能,但在极端条件下稳定性仍不够。在90℃存放500小时后,起偏振镜对于非偏振光的透光度发生变化,透光度的变化ΔTunpol大于5%。
然而,只有在这些条件下起偏振镜的光学性能的降低ΔTunpol和ΔP(ΔP为偏振化角度的变化)不超过5%,才有可能将其用于暴露在特别高的温度下的光学显示(例如汽车的仪表盘)。据报导,例如POLPAC起偏振镜粘合在玻璃板之间后,在100℃保持1,000小时其光学性能不变。然而,这样的层压体系不很适合于显示器的生产。从加工性能和挠性塑料显示器两者的角度来看,优选挠性起偏振镜。
因此,本发明的目的是制造满足上述条件的、基于具有共轭双键的聚合物的起偏振镜。
我们现在惊讶地发现,如果用SiOx层密封起偏振镜的表面则可达到这一目的。
本发明的密封是通过物理汽相淀积(PVD)、通过等离子化学汽相淀积(等离子CVD)或通过喷镀进行的。这些方法及其变异的方法是本领域技术人员已知的。优选使用PVD法。
在用PVD法进行密封时,在没有或有不同量的O2的条件下将市售SiO蒸发并淀积到待密封的起偏振镜上。在不存在O2的条件下,可获得SiO保护层;在有O2的条件下,保护层的氧气含量增加直至最终;在过量O2的存在下,淀积一层SiO2。x为1-2的SiOx代表了这一范围。为使起偏振镜对氧气稳定化,x值优选1.1-1.9,特别是1.4-1.8。然而,x高达2的值可用来获得机械性能(例如抗刮伤性)。
类似地,也可用等离子CVD法来达到密封。在这种情况下,通过例如硅烷与O2源(如N2O或其它氧化氮)的化学反应和淀积得到在待密封的起偏振镜上的SiOx保护层。
一种变异的方法是,首先由相对贫氧的SiOx(其中x=1.1-1.8)然后再由相对富氧的SiOx(其中x=1.4-2)可成功地建立保护层。
SiOx保护层的厚度为10nm至10μm,优选100nm至1μm。为进一步稳定化,也可将切割边用上述方法密封。
本发明还涉及包括具有共轭双键的聚合物起偏振芯层和两面均具有透明的挠性外层的层压的挠性起偏振镜,其特征在于芯层用SiOx保护层密封,外层用硅酸盐层或者用有机粘合剂粘合,用这种方式层压的起偏振镜是挠性的。借助于硅酸盐层,该起偏振镜也可用来粘在玻璃板、光学透镜或棱镜上。如果起偏振镜的一面通过硅酸盐层或通过有机粘合剂粘在玻璃显示器或其它玻璃元件上,则用SiOx层足以保护其游离表面。
这类硅酸盐层最好以水溶液的形式涂覆在用SiOx保护层密封的芯层上和/或外层上。适当的硅酸盐水溶液是已知的钠水玻璃和钾水玻璃的水溶液。常规类型的水玻璃,对于钠水玻璃而言,固体含量为25-60%(重量),二氧化硅含量为20-40%(重量);其余所含的固体是Na2O;对于钾水玻璃而言,固体含量为25-40%(重量),二氧化硅含量为20-30%(重量);其余所含的固体是K2O。为获得较薄的硅酸盐层,也可用水稀释这些溶液。二氧化硅的含量最好尽可能高,即SiO2/Na2O重量比≥3或SiO2/K2O重量比≥2.2。硅酸盐层的使用使US 5,049,427中所述的大量有机粘合剂成为不必要。
硅酸盐层仅以≤2μm的厚度与SiOx层一起使起偏振镜的性能稳定化。为达到层压制品的热稳定性粘合,每平方米待粘合表面需要100毫克至2克水玻璃(固体)。
在一个优选的实施方案中,在用硅酸盐溶液涂覆之前,将SiOx密封的芯层和/或外层用硅烷或硼酸盐处理。这一措施尤其可以提高粘合强度。
适宜的硅烷的化学式如下:
Si(R1)n(R2)4-n式中
R1各自独立地是卤素或烷氧基,
R2各自独立地是烷基或链烯基,
n是数字2,3或4。烷基和烷氧基基团R1和R2可以是被取代的。
适宜的硅烷的例子是四甲氧基硅烷、四乙氧基硅烷、甲基三甲氧基硅烷、二甲基二甲氧基硅烷、乙基三乙氧基硅烷、二甲基二氯硅烷、乙烯基甲基二氯硅烷和乙烯基三乙氧基硅烷。也可以将硅烷直接(例如乳化)混入硅酸盐溶液中。
适宜的硼酸盐的例子是硼酸和硼砂。也可以将硼酸和硼酸盐直接混入水玻璃溶液中或者溶于其中。
硅烷和硼酸盐特别是通过将SiOx密封的芯层和/或外层浸入该化合物的溶液中,或者如果化合物是溶液,则浸入纯化合物中然后再将其取出。所吸收的量是如此之小,以至于不能够通过称重法可靠地测量出来,但通常低于1克/平方米。
外层的厚度为例如5μm至1mm,优选20-200μm。偏振芯层的厚度为例如1-200μm,优选5-50μm。
适宜的外层的例子有:芳族聚酯、聚丙烯腈、聚(甲基)丙烯酸酯、聚砜、芳族聚碳酸酯、醋酸纤维素、乙酰丁酸纤维素、聚酰胺、聚己内酰脲、聚酰亚胺、聚酰胺酰亚胺、聚对亚苯基苯并二咪唑和聚对亚苯基苯并二噁唑和聚醚酮,优选聚酯、聚(甲基)丙烯酸酯、聚碳酸酯和纤维素酯。这些材料最重要的特性是其透明性。它们通常以薄膜的形式使用。
本发明的表面用SiOx密封的起偏振镜的偏振芯层是具有共轭双键的聚合物,这样的聚合物是已知的。例如,US 3,914,017描述了聚乙烯醇的部分脱水,从而导致聚合物主链中共轭双键微区的形成。这样产生的共轭双键微区通常相当短(平均:2-15 C=C)。脱水可以纯粹用热来进行,也可以用酸催化剂进行。待水解的聚乙烯醇可以用乙烯基单体接枝,例如用(甲基)丙烯酸酯、丙烯腈、苯乙烯、醋酸乙烯酯或氯乙烯接枝。类似地,共轭双键可通过从聚氯乙烯中脱除HCl或通过从聚乙酸乙烯酯中脱除乙酸而形成。上述含PAC聚合物可通过乙炔在聚合物中的聚合而不是PAC在溶液中的聚合形成。所有这些聚合物都可用于本发明。
偏振芯层最好是部分水解的聚乙烯醇或PAC。
偏振芯层特别优选是由含PAC聚合物产物制得的起偏振镜,其基体是含有极性基团的聚合物,其最大偏振程度P至少为90%,优选至少为95%,特别优选至少98%,最大二色性比QE不小于5,优选不小于10,上述两种情况均基于可见光计。这些起偏振镜以具有拉伸产生的优先方向的薄膜的形式使用。拉伸程度ε大于200%,优选至少400%,特别优选500-1,000%。
特别优选的偏振芯层由含PAC聚合物产物组成,其基体是部分水解的聚乙烯醇,其偏振效应从不可见的近紫外波长区(小于450nm)经过可见波长区(450-700nm)到近红外区(700-850nm)。可以制备这样的部分脱水的POLPAC起偏振镜:a)在进行乙炔聚合之前,将所用的聚乙烯醇在150-250℃回火,直至达到所需的脱水,这可通过褪色看出,然后在这样处理的聚乙烯醇溶液中将乙炔聚合,从而制得薄膜并拉伸之;或者b)将基体是聚乙烯醇的POLPAC薄膜拉伸然后回火,该回火可以在有或无空气存在下进行以保持长波偏振效果。也可以在拉伸之前或之后用酸例如HCl气体将薄膜预处理以促进水解过程。类似地,也可以在制成薄膜之前向聚合物中加入少量酸,例如盐酸、磷酸、硫酸或含硫酸的物质。
线型偏振光的偏振程度P和拉伸程度ε的定义如下: (l=拉伸后的长度;l0=拉伸前的长度)
含PAC聚合物产物被披露于例如US 5,049,427中,其中乙炔是在适宜的催化剂存在下,例如在非PAC的聚合物的溶液中的Ni(O)配合物存在下,在聚合物溶液中聚合的。
非PAC聚合物的量,基于起偏振镜的总量计,为1-99.9%(重量),优选50-99.9%(重量)。
适宜的非PAC聚合物的例子是聚氯乙烯、聚丁酸乙烯酯、聚乙烯醇、部分水解的聚乙酸乙烯酯(PVAC)和其它含乙烯醇的(共)聚合物、聚丙烯腈、含丙烯腈共聚物、聚乙烯基吡咯烷酮、甲基纤维素和其它纤维素衍生物,和聚碳酸酯。优选PVA和部分水解的PVAC的溶液。
非PAC聚合物的溶剂的例子包括N-甲基吡咯烷酮(NMP)、二甲基甲酰胺(DMF)和二甲基亚砜(DMSO)。溶剂中聚合物的浓度为1-20%(重量),优选2-20%(重量)。
新的层压起偏振镜明显地具有许多优异的性能:1.高的透光度2.高的光牢度3.耐热的偏振芯层4.极佳的机械性能
本发明的新的起偏振镜适用于所有使用偏振薄膜的领域,特别是光学用品(例如偏光显微镜、照相术和太阳镜的抗反射涂层和滑雪护目镜)和用于液晶显示,例如,用于手表、袖珍计算器、laptops、计算机、投影显示器、视频游戏、camcorders和平面屏幕电视机。
在80℃,即使未层压的不含稳定剂的POLPAC薄膜也具有良好的稳定性,透光度的变化(ΔT)在80℃在空气中500小时后为2-3%,而偏振程度的变化(ΔP)则小于1%。
该新的起偏振镜除了含有具共轭双键的聚合物(例如聚乙炔)之外,还可含有二色性物质,例如碘或二色性染料。然而,聚乙炔占二色性物质总量的至少50%(重量),优选至少80%(重量)。
实施例1
拉伸700%的厚度为11μm的POLPAC薄膜在600nm处的透光度T为38.7%,偏振程度P为99.99%。在80℃下500小时后,透光度升至41.7%,而偏振程度仅降低至99.89%。
实施例2
将与实施例1相同的薄膜在90℃保温,即使经过270小时后,在这期间在600nm处的透光度上升5.1%点,偏振程度降低1.84%点。
实施例3
将拉伸600%、尺寸为60mm×60mm的类似于实施例1的薄膜试样接到在A1100型汽相淀积装置(Leybold-Heraeus,Hanau,BRD)中的可旋转底材支架上。然后关闭汽相淀积装置的加工室并抽真空至大约10-3Pa。然后引入氧气至压力达7Pa,开动底材支架的旋转驱动装置,使支架以20转/分钟的速率旋转。通过给作为阴极连接的铝板施加相对于地球为-480V的电压引发低压等离子体。以5.6瓦的功率将一样在该等离子体中处理2分钟。然后关掉电压,停止加入氧气,将加工室抽真空至10-4Pa。
达到该压力后,重新将氧气引入加工室中直至获得10-2Pa的压力。达到该压力后,打开电子束枪,以400W的功率在4分钟内将水冷却的铜坩锅中的待蒸发的SiO(商品名Patinal,Merck,Darmstadt)加热至大约1950K。随后去掉电子束枪与底材支架之间的可移动隔膜,将薄膜片以0.5nm/秒的速率涂覆400秒。然后将隔膜再次置于电子束枪与底材支架之间,停止加入氧气并终止涂覆过程。关掉电子束枪并将蒸发材料冷却之后,释放加工室中的真空。取出一面涂覆的薄膜,翻转,再如上述那样对未涂覆面进行汽相淀积。
将两面均涂覆SiOx(每面的厚度为200nm)的薄膜不经过层压,进行90℃加热试验,在这期间,480小时后透光度仅增加2.1%(从33.3%到35.4%)。偏振程度的降低仅为0.5%(从99.8%到99.3%),两者均在600nm处测定。
实施例4
用拉伸600%的脱水和接枝聚乙烯醇薄膜重复实施例3。用于该薄膜的聚合物是通过用丙烯酸乙酯和甲基丙烯酸甲酯接枝聚乙烯醇随后用无水氯化氢脱除水分子而制得的。每面的SiOx涂层的厚度为180nm。在加热试验期间,透光度仅改变2%,偏振程度仅改变1%,两者均在600nm处测定。
实施例5
将23μm厚的聚乙烯醇(由聚乙酸乙烯酯的皂化制得;皂化度:99%)薄膜在室温下暴露在氯化氢气氛中5分钟,然后在200℃单轴拉伸7倍,在200℃拉伸张力下再保持15分钟。这时薄膜厚度为12μm。用偏振光测定得到43.9%的透光度和93.9%的偏振程度。用实施例3的方法用SiOx(x=1.7)涂覆薄膜。在90℃的加热试验后的重复测定结果是:透光度改变小于2%,偏振程度改变0.9%。
实施例6
用气态氯化氢处理POLPAC薄膜,并在氩气氛中拉伸700%,即拉伸至其原长度的8倍,然后在200℃的空气中回火15分钟。在600nm处的透光度为38.5%,偏振程度为99.99%。在400nm处由于回火的偏振效应从81%上升到96%。在700nm处的偏振效应仅从99.8%降至98.1%。在用SiOx涂覆并在90℃进行20天的加热试验后,透光度改变小于2%,偏振程度改变小于1%。若回火是在氩气氛中进行的,则在700nm处观察不到偏振的改变。
Claims (10)
1.包括具有共轭双键的聚合物起偏振层的耐热的挠性起偏振镜,其特征在于:它具有SiOx密封表面,其中x是1-2的任意值,优选1.1-1.9,特别优选1.4-1.8。
2.根据权利要求1的起偏振镜,其特征在于:用SiOx对表面的密封是通过物理汽相淀积(PVD)、等离子化学汽相淀积(等离子CVD)或喷镀进行的,优选通过PVD进行。
3.根据权利要求2的起偏振镜,其特征在于:SiOx保护层的厚度为10nm至10μm,优选100nm至1μm。
4.根据权利要求1的起偏振镜,其特征在于:它还包括贴在两边的透明的挠性外层,所述外层是用硅酸盐或有机粘合剂、优选硅酸盐粘合到SiOx层上的。
5.根据权利要求4的起偏振镜,其特征在于:在将SiOx密封的起偏振层和/或外层用硅酸盐溶液涂覆前用硅烷或硼酸盐处理。
6.根据权利要求4的起偏振镜,其特征在于:将硅酸盐溶液与硅烷和/或硼酸盐混合。
7.根据权利要求5的起偏振镜,其特征在于:硅烷的化学式为:
Si(R1)n(R2)4-n式中
R1各自独立地是卤素或烷氧基,
R2各自独立地是烷基或链烯基,
n 是数字2,3或4。
8.根据权利要求1的起偏振镜,其特征在于:聚合物是部分脱水的聚乙烯醇或含有聚乙烯醇的聚乙炔,优选含有聚乙烯醇的聚乙炔。
9.根据权利要求1的起偏振镜,其特征在于:它含有外加的二色性的物质。
10.根据权利要求8的起偏振镜,其特征在于:聚合物是含有聚乙烯醇的聚乙炔,该聚乙烯醇在乙炔聚合之前或之后通过在150-250℃回火、通过酸处理或通过回火和酸处理进行部分脱水。
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CN107561619A (zh) * | 2016-06-30 | 2018-01-09 | 乐金显示有限公司 | 偏振器、具有偏振器的显示装置以及偏振器的制造方法 |
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US6808657B2 (en) * | 2002-02-12 | 2004-10-26 | 3M Innovative Properties Company | Process for preparing a K-type polarizer |
US7087194B2 (en) * | 2002-04-04 | 2006-08-08 | 3M Innovative Properties Company | K-type polarizer and preparation thereof |
US6949207B2 (en) * | 2002-04-04 | 2005-09-27 | 3M Innovative Properties Company | K-type polarizer and preparation thereof |
JP4149201B2 (ja) * | 2002-06-12 | 2008-09-10 | 株式会社クラレ | 偏光フィルムの製造法 |
US7122234B2 (en) * | 2002-11-13 | 2006-10-17 | Tetra Laval Holding & Finance S.A. | Transparent plastic gas barrier packaging laminate |
JP2006315364A (ja) * | 2005-05-16 | 2006-11-24 | Univ Nagoya | 複合フィルムおよびその製造方法 |
DE102010043200A1 (de) * | 2010-02-10 | 2011-08-11 | Johnson Controls Automotive Electronics GmbH, 75196 | Anzeigeelement für eine Anzeigeeinheit in einem Fahrzeug |
JP2015034848A (ja) * | 2013-08-07 | 2015-02-19 | チェイル インダストリーズ インコーポレイテッド | ポリエン(polyene)系偏光フィルム(film)の製造方法、ポリエン系偏光フィルム、積層偏光フィルム、及び表示装置 |
JP6585333B2 (ja) * | 2013-12-03 | 2019-10-02 | 日東電工株式会社 | 偏光フィルム、粘着剤層付偏光フィルムおよび画像表示装置 |
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DE3842968A1 (de) * | 1988-12-21 | 1990-06-28 | Bayer Ag | Laminierte polarisatoren |
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CN103183964A (zh) * | 2013-04-02 | 2013-07-03 | 深圳市华力兴工程塑料有限公司 | 一种导热复合材料及其制备方法 |
CN103183964B (zh) * | 2013-04-02 | 2015-06-10 | 深圳华力兴新材料股份有限公司 | 一种导热复合材料及其制备方法 |
CN107561619A (zh) * | 2016-06-30 | 2018-01-09 | 乐金显示有限公司 | 偏振器、具有偏振器的显示装置以及偏振器的制造方法 |
US10429550B2 (en) | 2016-06-30 | 2019-10-01 | Lg Display Co., Ltd. | Polarizer having adhesive-covered polarizing layer, display device having the polarizer, and method of fabricating the polarizer |
Also Published As
Publication number | Publication date |
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FI960377A (fi) | 1996-07-31 |
EP0724024A1 (de) | 1996-07-31 |
FI960377A0 (fi) | 1996-01-26 |
CN1083987C (zh) | 2002-05-01 |
EP0724024B1 (de) | 1999-05-12 |
DE59601846D1 (de) | 1999-06-17 |
KR100394204B1 (ko) | 2004-01-07 |
US5705267A (en) | 1998-01-06 |
JPH08262228A (ja) | 1996-10-11 |
TW282519B (zh) | 1996-08-01 |
KR960029090A (ko) | 1996-08-17 |
CA2168180A1 (en) | 1996-07-31 |
DE19502806A1 (de) | 1996-08-01 |
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