CN1293131C - 层压聚酯薄膜和层压薄膜 - Google Patents
层压聚酯薄膜和层压薄膜 Download PDFInfo
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- CN1293131C CN1293131C CNB038128713A CN03812871A CN1293131C CN 1293131 C CN1293131 C CN 1293131C CN B038128713 A CNB038128713 A CN B038128713A CN 03812871 A CN03812871 A CN 03812871A CN 1293131 C CN1293131 C CN 1293131C
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- Prior art keywords
- film
- laminated
- laminated polyester
- polyester film
- coating
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Abstract
提供一种滑动性、透明性、尺寸稳定性、耐冲击性、粘合性优异的层压聚酯薄膜,其特征在于包含一种由聚酯构成、在至少一个方向上拉伸的基材薄膜和在其至少一面上施用的涂层,该涂层包含高分子粘结剂和微粒,该微粒的折射率与高分子粘结剂的折射率实质上相同,进而层压聚酯薄膜的光雾度在1.5%以下、全光线透射率在85%以上、每100μm薄膜厚度的50%断裂能为0.3J以上、在230℃ 30分钟条件下的热收缩率在4%以下。
Description
技术领域
本发明涉及包含在至少一个方向上拉伸的聚酯基材薄膜和在其至少一面上设置的涂层的层压聚酯薄膜和使用此层压薄膜的层压薄膜。
背景技术
聚酯薄膜由于有优异的机械性质、耐热性、及耐药品性而可用作为磁带、强磁性薄膜带、照相胶片、包装用薄膜、电子零件用薄膜、电绝缘薄膜、金属层压用薄膜、各种零件材料的保护用薄膜等等。近年来,也使用在图像显示装置的显示面板上。图像显示装置如液晶显示装置的显示面板虽然一直采用玻璃基板但近年来随着图像显示装置的薄型化、轻量化、以及大画面化的进展,正在探讨使用聚酯薄膜的可行性。
发明公开
到目前为止一直非常难以获得具备充分耐冲击性、透明性、以及滑动性、同时对粘合剂层或硬涂层的粘合性优异的高分子薄膜。图像显示装置的显示面板上使用的高分子薄膜,因用途而异,可以层压气体阻透层、导电体层、半导体层、发光体层等功能层。这些功能层是以蒸气沉积、离子镀、溅射、等离子体CDV等方法层压的,因而高分子薄膜在层压步骤中曝露颇高的温度。因此,在功能层层压于高分子薄膜上的层压步骤中或层压步骤后,要么得到龟裂、皱纹的层压体,要么得到断裂的层压体,有不能发挥作为层压体的功能的问题。
本发明以解决这样的先有技术问题并得到兼备充分耐冲击性、透明性以及滑动性,同时对粘合剂层或硬涂层的粘合性优异、进而尺寸稳定性、耐冲击性优异的层压聚酯薄膜为课题。
按照本发明,上述课题可以用一种层压聚酯薄膜解决,其特征在于包含在至少一个方向上拉伸的聚酯基材薄膜,与在其至少一面上设置的涂层;该涂层含有高分子粘结剂和微粒,该微粒的折射率与高分子粘结剂的折射率实质上相同;进而,层压聚酯薄膜的光雾在1.5%以下、全光线透射率在85%以上、薄膜厚度100μm时的50%断裂能在0.3J以上,在230℃30分钟的条件下的热收缩率在4%以下。
以下详细说明本发明。
<基材薄膜>
本发明中,构成基材薄膜的聚酯,是从芳香族二元酸或其酯形成性衍生物与二醇类或其酯形成性衍生物形成的线型饱和聚酯。这样的聚酯的具体例,可以列举聚对苯二甲酸乙二醇酯,聚间苯二甲酸乙二醇酯,聚对苯二甲酸丁二醇酯,聚(对苯二甲酸1,4-环己烷二甲酯),聚-2,6-萘二羧酸乙二醇酯等。这些聚酯中,就力学物性或光学物性的平衡的观点而言,以聚对苯二甲酸乙二醇酯、聚-2,6-萘二羧酸乙二醇酯较为适用;就机械强度高、热收缩率小、加热时低聚物发生量少的观点而言,以聚-2,6-萘二羧酸乙二醇酯较为适合。
聚酯是均聚物、共聚物皆可。在使用共聚物作为聚酯时,构成共聚物的共聚酸成分,可以列举苯二甲酸,2,6-萘二羧酸等芳香族二羧酸;己二酸、壬二酸、癸二酸、1,10-癸烷二羧酸等脂肪族二羧酸。二醇成分可以列举1,4-丁二醇、1,6-己二醇、新戊二醇等脂肪族二醇;1,4-环己烷二甲醇等脂环族二醇。这些既可以单独使用,也可以使用两种以上。
聚酯既可以是诸如用苯甲酸、甲氧基聚(亚烷基)二醇等单官能性化合物封闭末端羟基及/或羧基的一部或全部者;也可以是以极少量诸如甘油、季戊四醇等三官能以上酯形成性化合物在可得到实质上线型聚合物范围内进行共聚者。
本发明中,作为基材薄膜的聚酯,较好者之一是间苯二甲酸共聚的聚对苯二甲酸乙二醇酯;此间苯二甲酸共聚之聚对苯二甲酸乙二醇酯中对苯二甲酸相对于总二羧酸成分而言较好是90摩尔%以上、更好95摩尔%以上。因而,间苯二甲酸相对于总二羧酸成分而言较好是10摩尔%以下、更好5摩尔%以下。
本发明中,作为基材薄膜的聚酯,较好者之一是聚萘二羧酸乙二醇酯,特别好的是聚-2,6-萘二羧酸乙二醇酯;此聚-2,6-萘二羧酸乙二醇酯中2,6-萘二羧酸成分相对于总二羧酸成分而言较好是90摩尔%以上、更好95摩尔%以上、特别好97摩尔%以上。
本发明中的聚酯可依已往众所周知的方法制得。如二羧酸与二醇的反应可直接得到聚合度较低的聚酯。又,以二羧酸低级烷酯与二醇使用酯交换催化剂进行酯交换反应之后,在缩聚合催化剂的存在下进行聚合反应的方法也可制得聚酯。作为酯交换反应催化剂,可以使用含有例如钠、钾、镁、钙、锌、锶、钛、锆、锰、钴的化合物。作为缩聚催化剂,可以使用三氧化锑、五氧化锑等的锑化合物;以二氧化锗为代表的锗化合物;酞酸四乙酯、酞酸四丙酯、酞酸四苯酯或这些的部分水解物;草酸氧钛铵、草酸氧钛钙、三乙酰丙酮钛等钛化合物。在经由酯交换反应进行缩聚反应时,较好使酯交换反应催化剂在缩聚反应之前失活;这种失活通过将磷酸三甲酯、磷酸三乙酯、磷酸三正丁酯、正磷酸等磷化合物,以磷元素计相对于聚酯而言20~100ppm添加即可。聚酯也可实施固相聚合,此时将熔融聚合所得的聚酯切片、在加热减压下或氮气等惰性气流下进行固相聚合。
聚酯的特性粘度较好在0.40dl/g以上,更好0.40~0.90dl/g。特性粘度低于0.40dl/g时,会频繁发生工艺断裂,因而不好。高于0.90dl/g时,熔融粘度高而难以熔融挤出而且聚合时间长而不经济因而不好。聚酯中也可以含有着色剂、防静电剂、抗氧剂、有机滑剂等。
<涂层>
本发明的层压聚酯薄膜中,在上述基材薄膜的至少一面上设置了涂层。此涂层包含高分子粘结剂及微粒。此微粒的折射率与高分子粘结剂的折射率实质上相同。折射率实质上相同系指两者的折射率差在0.04以下。两者的折射率差较好小于0.02,更好小于0.01,特别好小于0.005。折射率差超过0.04时,由于高分子粘结剂与微粒之间界面的折射率差而使光线大量散射,以致涂层的光雾度升高、透明性恶化。
<高分子粘结剂>
高分子粘结剂,从给予良好粘合性的观点来看,较好是聚酯树脂和有唑啉基与聚烯化氧链的丙烯酸树脂的混合体。高分子粘结剂,虽以水可溶性或水分散性者为宜,但较好可以使用可溶于含有若干有机溶剂的水中者。本发明中涂层的高分子粘结剂的折射率通常在1.50~1.60的范围内。
<聚酯树脂>
构成高分子粘结剂的聚酯树脂,可以使用从下列多元酸成分与二醇成分得到的聚酯;即,多元酸成分可以列举诸如对苯二甲酸、间苯二甲酸、邻苯二甲酸、邻苯二甲酸酐、2,6-萘二羧酸、1,4-环己烷二羧酸、己二酸、癸二酸、偏苯三酸,均苯四甲酸,二聚物酸,5-钠磺基间苯二甲酸。构成高分子粘结剂的聚酯树脂,较好使用由两种以上二羧酸成分共聚的聚酯。聚酯树脂中,可以含有若干量的马来酸、衣康酸等不饱和多元酸、或对-羟基苯甲酸等的羟基羧酸。
聚酯树脂的二醇类成分可以列举乙二醇、1,4-丁二醇、二甘醇、二聚丙二醇、1,6-己二醇、1,4-环己烷二甲醇、苯二甲醇,二(羟甲基)丙烷等或聚(环氧乙烷)二醇、聚(四氢呋喃)二醇等。
高分子粘结剂的聚酯树脂的玻璃化温度较好是40~100℃、更好60~80℃。于此范围内,可获得优异的粘合性及优异的耐损伤性。另一方面,玻璃化温度低于40℃时薄膜与薄膜之间容易发生粘连,超过100℃时涂膜会变得又硬又脆,使耐损伤性恶化而不佳。
<丙烯酸树脂>
作为可用来作为高分子粘结剂构成成分的有唑啉基和聚烯化氧链的丙烯酸树脂,可以使用例如以下所示有唑啉基的单体和有聚烯化氧链的单体形成的丙烯酸树脂。
有唑啉基的单体,可以列举2-乙烯基-2-唑啉,2-乙烯基-4-甲基-2-唑啉,2-乙烯基-5-甲基-2-唑啉,2-异丙烯基-2-唑啉,2-异丙烯基-4-甲基-2-唑啉,2-异丙烯基-5-甲基-2-唑啉。可以使用其中一种或两种以上的混合物。其中,2-异丙烯基-2-唑啉是工业上容易得到的,因而较适用。使用有唑啉基的丙烯酸树脂可以提高涂层的凝聚力,并使其与硬涂层或粘合层等的粘合性更牢固。进而还可以赋予薄膜以制膜步骤中及硬涂层加工步骤中对金属辊筒的耐擦伤性。
作为有聚烯化氧链的单体,可以列举在丙烯酸、甲基丙烯酸的酯部上加成了聚烯化氧者。聚烯化氧链可以列举聚甲醛、聚环氧乙烷、聚环氧丙烷、聚环氧丁烷。聚烯化氧链的重复单元以3-100为宜。使用有聚烯化氧链的丙烯酸树脂时,涂层高分子粘结剂中聚酯树脂与丙烯酸树脂的相溶性,较不含聚烯化氧链的丙烯酸树脂为佳,因而可提高涂层的透明性。聚烯化氧链的重复单元低于3时,聚酯树脂与丙烯酸树脂的相溶性不良,以致涂层的透明性恶化;而当超过100时,涂层的耐湿热性下降,从而在高湿度及高温下与硬涂层等的粘合性恶化,因而不好。
丙烯酸树脂中可以共聚诸如以下列举的单体作为其它共聚成分。即,丙烯酸烷酯、甲基丙烯酸烷酯(烷基为甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、2-乙基己基、环己基等);丙烯酸2-羟基乙酯、甲基丙烯酸2-羟基乙酯、丙烯酸2-羟基丙酯、甲基丙烯酸2-羟基丙酯等含羟基单体;丙烯酸环氧丙酯、甲基丙烯酸环氧丙酯、烯丙基环氧丙基醚等含环氧基单体;丙烯酸、甲基丙烯酸、衣康酸、马来酸、富马酸、巴豆酸、苯乙烯磺酸及其盐类(钠盐、钾盐、铵盐、叔丁胺盐等)等有羧基或其盐的单体;丙烯酰胺、甲基丙烯酰胺、N-烷基丙烯酰胺、N-烷基甲基丙烯酰胺、N,N-二烷基丙烯酰胺、N,N-二烷基甲基丙烯酰胺(烷基为甲基、乙基、正丙基、异丙基、正丁基、异丁基、叔丁基、2-乙基己基、环己基等)、N-烷氧基丙烯酰胺、N-烷氧基甲基丙烯酰胺、N,N-二烷氧基丙烯酰胺、N,N-二烷氧基甲基丙烯酰胺(烷氧基为甲氧基、乙氧基、丁氧基、异丁氧基等)、丙烯酰基吗啉、N-(羟甲基)丙烯酰胺、N-(羟甲基)甲基丙烯酰胺、N-苯基丙烯酰胺、N-苯基甲基丙烯酰胺等有酰胺基的单体;马来酸酐、衣康酸酐等酸酐单体;异氰酸乙烯酯、异氰酸烯丙酯、苯乙烯、α-甲基苯乙烯、乙烯基甲基醚、乙烯基乙基醚、乙烯基三烷氧基甲硅烷、马来酸单烷酯、富马酸单烷酯、衣康酸单烷酯、丙烯腈、甲基丙烯腈、偏二氯乙烯、乙烯、丙烯、氯乙烯、乙酸乙烯酯,丁二烯。
<高分子粘结剂的量比>
形成涂层的聚酯树脂在涂层中的含有比例以5~95重量%为宜、以50~90重量%为最佳。形成涂层的含唑啉基及聚烯化氧链的丙烯酸树脂在涂层中的含有比例以50~90重量%为宜、以10~50重量%为最佳。聚酯树脂超过95重量%、或含唑啉基与聚烯化氧链的丙烯酸树脂低于5重量%,涂层的凝聚力下降,有时对硬涂层或粘合剂的粘合性不足,因而不好。丙烯酸树脂超过90重量%时,与聚酯薄膜的粘合性将下降,有时对硬涂层或粘合剂的粘合性不足,因而不好。
<微粒>
本发明中构成涂层的微粒以使用二氧化硅与二氧化钛的复合无机微粒为佳。此二氧化硅与二氧化钛的复合无机微粒有任意地进行折射率调整的可能,因而,可容易地调整其折射率。由于高分子粘结剂的折射率在1.50~1.60范围内,因而可以容易地整合高分子粘结剂与微粒的折射率。微粒的折射率亦以在和高分子粘结剂相同的1.50~1.60的范围内为佳。
微粒的平均粒径以40~120nm的范围为宜;大于120nm时微粒容易发生脱落,小于40nm时有时不能获得充分的滑动性及耐损伤性,因而都不好。微粒的含有量以在涂层的0.1~10重量%的范围为佳;低于0.1重量%时不能获得充分的滑动性及耐损伤性,超过10重量%时涂膜的凝聚力下降、粘合性恶化,因而不好。
<脂肪族蜡>
涂层中含有脂肪族蜡可使薄膜的表面获得滑动性,因而较好;其含有量以0.5~30重量%为宜,以1重量%~10重量%更佳。此含有量低于0.5重量%时薄膜表面的滑动性不足,因而不好;超过30重量%时对聚酯薄膜基材的粘合或对硬涂层或粘合剂的易粘附性有时不足,因而不好。脂肪族蜡的具体例可以列举巴西棕榈蜡、小烛树脂、米蜡、木蜡、霍霍巴油、棕榈蜡、松香改性蜡、小冠椰子蜡、甘蔗蜡、西班牙草蜡、树皮蜡等植物系蜡,蜂蜡、羊毛脂、鲸蜡、白蜡、虫胶蜡等动物系蜡,褐煤蜡、天然地蜡、纯地蜡等矿物系蜡,石蜡、微晶蜡、矿脂等石油系蜡,费托合成蜡、聚乙烯蜡、氧化聚乙烯蜡、聚丙烯蜡、氧化聚丙烯蜡等合成烃系蜡;其中,由于对硬涂层及粘合剂等的易粘附性及滑动性良好,因而巴西棕榈蜡,石蜡,聚乙烯蜡最为适合。这些可以降低环境荷载且较好作为容易操作的水分散体使用。
<添加剂>
为进一步提高涂层的滑动性及耐损伤性,在不影响透明性的情况下也可以含有其他微粒。其它微粒可以列举诸如碳酸钙、碳酸镁、氧化钙、氧化锌、氧化镁、二氧化硅、硅酸钠、氢氧化铝、氧化铁、氧化锆、硫酸钡、二氧化钛、氧化锡、三氧化锑、碳黑、二硫化钼等无机微粒或丙烯酸系交联聚合物、苯乙烯系交联聚合体、硅酮树脂、氟树脂、苯并鸟嘌呤胺树脂、苯酚树脂、尼龙树脂等有机微粒;这些当中,为避免水不溶性固体物质在水分散液中沉淀,以选择比重不超过3的微粒为佳。
<层压聚酯薄膜的物性>
本发明的层压聚酯薄膜,具备或较好具备下列各特性。
<光雾度>
本发明的层压聚酯薄膜的光雾度必须在1.5%以下。光雾度超过1.5%时透明性不佳、辉度下降,因而难以用于显示器上;光雾度在1.0%以下更佳、在0.5%以下最为适合。
<全光线透射率>
本发明的层压聚酯薄膜的全光线透射率必须在85%以上。全光线透射率不足85%时透明性不佳、辉度下降,因而难以用于显示器上。全光线透射率在87%以上更佳、在90%以上最为适用。
<50%断裂能>
本发明的层压聚酯薄膜在厚度100μm时的50%断裂能必须在0.3J以上。厚度100μm时的50%断裂能不足0.3J时其耐冲击性不佳、容易破裂,因而难以用于可挠曲显示器用途。厚度100μm时的50%断裂能在0.4J以上更佳、在0.5J以上最为适用。
<热收缩度>
本发明的层压聚酯薄膜在230℃30分钟的条件下的热收缩率必须在4%以下。此热收缩率超过4%时,在功能层层压于薄膜上之时或层压之后,层压体上会产生龟裂及皱纹,从而破坏层压体,导致不能充分发挥其功能。热收缩率在2%以下更佳、在1%以下最为适用。
<表面糙度>
本发明的层压聚酯薄膜的薄膜表面三维中心线平均糙度SRa是任何一面上都以2~20nm为宜。SRa小于2nm时不能获得充分的易滑性,很难卷取。而超过20nm时虽然易滑性优越,但在功能膜层压于薄膜上时会发生涂层脱落或蒸气沉积层脱落而不能充分发挥其功能。
本发明的层压聚酯薄膜以至少单面的十点平均糙度Rz在50~150nm范围内为宜;Rz不足50nm时不能获得充分的易滑性,很难卷取,而超过150nm时虽然易滑性优异但在功能膜层压于薄膜上时会发生涂层脱落或蒸气沉积层脱落而不能充分发挥其功能。
<折射率指数>
本发明的层压聚酯薄膜在以连续制膜法制膜时连续制膜方向上的折射率为nMD,在与连续制膜方向垂直的方向上的折射率为nTD时,薄膜面方向的折射率差指数的绝对值以50以下为宜。此薄膜面方向的折射率指数以下式表示。
Δn=(nMD-nTD)×1000
此Δn以-50~50为宜,以-40~40更佳,以-30~30最好
Δn的绝对值超过50时,薄膜面方向的各向异性增大,热收缩率的各向异性也变大,在功能层层压时会在特定方向上产生龟裂及皱纹,从而不能充分发挥其功能,因而不好。
<杨氏模量>
本发明的层压聚酯薄膜的杨氏模量以3~15GPa为宜。不足3GPa时薄膜易伸长而不适于以辊筒操作;而超过15GPa时薄膜生产率不良。杨氏模量以4~12GPa为佳,在5~10GPa范围内最为适用。
<厚度>
本发明的层压聚酯薄膜在作为液晶、硬涂层、触摸板、防晕眩处理、等离子体显示板(PDP)用电磁屏蔽膜、有机电发光(EL)、电子纸张、太阳能电池等的支撑体使用时,为了得到必要的强度及一定程度的自由挠曲性,其厚度以12~500μm为宜、以25~350μm更佳、以50~250μm为最适用。又,本发明的层压聚酯薄膜要么不含充填剂,要么即使含有,较好也是少量不影响其特性的小粒径者。
<层压聚酯薄膜的制造方法>
本发明的层压聚酯薄膜可以诸如将上述聚酯熔融挤出成薄膜状、以流延辊筒冷却固化成为未拉伸薄膜,此未拉伸薄膜在玻璃化温度(Tg)~(Tg+60)℃进行纵向及横向的双轴拉伸,其倍率为2.0~5.0倍;并在(Tm-100)~(Tm-5)℃的温度下进行1~100秒钟热定形,得到所希望的薄膜。拉伸可以采用一般使用的方法例如辊筒法或展幅机法;既可以在纵向与横向上同时拉伸,也可以在纵向与横向上逐次拉伸。涂层在逐次拉伸的情况下可在一方向拉伸的单轴取向薄膜上涂布水性涂液之后直接进行另一方向拉伸,再经热定形即可。涂布方法可以使用辊涂法、照相凹版涂布法、辊刷法、喷涂法、气刀刮涂法、浸涂法、帘涂法等;这些方法可以单独或组合使用。上述Tg为聚合物的玻璃化温度,Tm为聚合物的熔点。
在进一步进行松弛处理时,在薄膜的(X-80)~X℃的温度下进行加热处理是有效果的;在此X表示热定形温度;松弛处理的方法有在热定形后至辊筒卷取之间的热定形区域途中将薄膜两端切离而使相对于薄膜的供给速度而言的拉取速度减慢的方法;在两个速度各异的传送辊之间以IR加热器加热的方法;在加热传送辊上传送薄膜而使加热传送辊后的传送辊减速的方法;边在热定形后吹送热风的喷嘴上方传送薄膜边将拉取速度减至低于供给速度的方法;或用制膜机卷取后以加热传送辊传送薄膜并使传送辊减速的方法;或者在加热炉内或IR加热器的加热区域传送,同时使加热区域后的辊速降到低于加热区域前的辊速的方法;可以使用其中任何一种方法;但较好以相对于供给侧的速度而言拉取侧速度的减速率为0.1~10%进行松弛处理。
特别对于本发明的涂层,由于使用具备上述特征的物质,因而可以制造出具有本发明必备特性的薄膜。
<层压薄膜>
本发明包含以下说明的形态作为较好实施形态。
<硬涂层>
本发明的层压聚酯薄膜也可在涂层之上设置硬涂层而成为有用的层压薄膜。硬涂层以使用耐药品性、耐损伤性强的硬化性树脂为佳。这样的硬化性树脂可以列举电离辐射硬化型树脂、热固型树脂、热塑性树脂等;其中以电离辐射硬化型树脂为佳。这是因为对透明基材薄膜的成膜作业容易进行,而且容易使铅笔硬度提高到所希望的值。
用于形成硬涂层的电离辐射硬化型树脂,以具有丙烯酸酯系官能基者为佳,以聚酯丙烯酸酯或聚氨酯丙烯酸酯最为适用。聚酯丙烯酸酯由聚酯系多醇的低聚物的丙烯酸酯和/或甲基丙烯酸酯〔以下称为(甲基)丙烯酸酯,包括丙烯酸酯与甲基丙烯酸酯〕构成。又,上述聚氨酯丙烯酸酯是由多醇化合物与二异氰酸酯化合物形成的低聚物经丙烯酸酯化的生成物构成的。构成丙烯酸酯的单体有(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸甲氧基乙酯、(甲基)丙烯酸丁氧基乙酯、(甲基)丙烯酸苯酯等。
在进一步提高上述硬涂层的硬度的情况下,可以并用多官能单体。具体的多官能单体,可以列举例如三(羟甲基)丙烷三(甲基)丙烯酸酯、己二醇(甲基)丙烯酸酯、三聚丙二醇二(甲基)丙烯酸酯、二甘醇二(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、二聚季戊四醇六(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、等。
用于形成硬涂层的聚酯系低聚物可以列举由己二酸与二醇类(乙二醇、聚乙二醇、丙二醇、丁二醇、聚丁二醇等)或三醇类(甘油、三(羟甲基)丙烷等)、癸二酸与二醇类或三醇类的缩合生成物的聚己二酸三醇酯、聚癸二酸多醇酯等。上述脂肪族二羧酸的一部分或全部也可以用其它有机酸代替。在这种情况下其它有机酸可以使用间苯二甲酸、对苯二甲酸、或邻苯二甲酸酐等;这些可使硬涂层具有极高的硬度,甚为适用。
用于形成硬涂层的聚氨酯系低聚物可由多异氰酸酯与多醇的缩合生成物得到。具体的多异氰酸酯可以列举亚甲基二(对苯二异氰酸酯)、六亚甲基二异氰酸酯·己三醇加成物、六亚甲基二异氰酸酯、甲苯二异氰酸酯、甲苯二异氰酸酯·三(羟甲基)丙烷加合物、1,5-萘二异氰酸酯、硫丙基二异氰酸酯、乙基苯-2,4-二异氰酸酯、2,4-甲苯二异氰酸酯二聚物,加氢二甲苯二异氰酸酯,硫代磷酸三(4-苯基异氰酸酯)酯等;又,具体的多醇类可以列举聚氧四亚甲基二醇等聚醚系多醇,聚己二酸酯多醇,聚碳酸酯多醇等聚酯系多醇,丙烯酸酯类与甲基丙烯酸羟乙酯的共聚物等。
更进一步,作为上述电离辐射硬化型树脂,当使用紫外线硬化型树脂时,较好在这些树脂中混合使用苯乙酮类、二苯甲酮类、米蚩苯甲酰苯甲酸酯、α-戊肟酯或硫呫吨酮类等作为光聚合引发剂,及正丁胺、三乙胺、三正丁膦等作为光增感剂等。
要说明的是,聚氨酯丙烯酸酯富于弹性或可挠性、加工性优异;其反面是表面硬度不足,难以达到2H以上的铅笔硬度。与此相反,聚酯丙烯酸酯可通过选择聚酯构成成分来形成硬度极高的硬涂层。因此,由于高硬度与可挠性容易形成对立,因而硬涂层的配合比较好是聚氨酯丙烯酸酯占60~90重量分、聚酯丙烯酸酯占40~10重量分。
形成上述硬涂层所使用的涂布液中,为了在调整光泽的同时赋予表面滑动性,较好相对于树脂成分100重量分而言添加二次粒径在20μm以下的惰性微粒0.3~3重量分。添加量在0.3重量分以下时,滑动性提高效果不足;另一方面,超过3重量分时所得硬涂层的铅笔硬度下降。涂布液中添加的惰性微粒可以列举二氧化硅、碳酸镁、氢氧化铝、硫酸钡等无机微粒,此外还可以列举聚碳酸酯、丙烯酸树脂、聚酰亚胺、聚酰胺、聚萘二甲酸乙二醇酯、三聚氰胺树脂等有机聚合物微粒。
又,硬涂层中还可以含有紫外线吸收剂。这样就可以防止透明基材及着色剂(特别是染料系着色剂)的紫外线劣化,并保持长时间视认性及防爆性。紫外线吸收剂的种类没有特别的限制,但较好选自上述特定的环状亚氨基酯。相对于形成硬涂层的树脂而言,添加量以0.1~10重量%为佳。低于0.1重量%时,对紫外线劣化的防止效果小;而超过10重量%时,耐磨耗性或耐擦伤性低下。添加的方法,以在溶剂中分散使用为佳。
用于形成硬涂层的涂布方法,因涂布液的特性及涂布量而异,可适当选择本身已知的惯常方法如辊涂法、照相凹版涂布法、棒涂法、挤出涂布法等。硬涂层的厚度没有特别的限制,以1~15μm的范围为佳。涂布液的固形分浓度以30~70重量%为宜,以40~60重量%更好。
硬涂层上设置的层压薄膜的构成,可以列举在本发明层压聚酯薄膜的涂层上设置硬涂层的构成、在涂层与基材薄膜两者之上设置硬涂层的构成、在涂层设置于基材薄膜两面的两涂层之上设置硬涂层的构成。按照本发明,也提供了这样的层压薄膜。
<气体阻透层>
本发明层压聚酯薄膜之上也可以设置气体阻透层而成为有用的层压薄膜。气体阻透层既可以直接设置在本发明层压聚酯薄膜的涂层之上;也可以设置于涂层与硬涂层之间。此外,还可以设置在与涂层相反一侧的基材薄膜上。在作为液晶显示板或有机电发光板的用途上,以设置气体阻透层为佳。气体阻透层也可以使用有机材料系及无机材料系中任何一种材料。
有机材料系的气体阻透层可以使用由聚乙烯醇、乙烯醇-乙烯共聚物等乙烯醇共聚物,聚丙烯腈,丙烯腈-丙烯酸甲酯共聚物或丙烯腈-苯乙烯共聚物等丙烯腈共聚物,或聚偏二氯乙烯等有机高分子材料组成的层。这些材料可借助于使用照相凹版涂布器或逆辊涂布器的湿式涂布法在本发明聚酯上形成气体阻透层。使用聚乙烯系阻透层时容易因吸湿而使氧气阻透特性急剧下降;因而较好还以其它方式形成水蒸气阻透层。
无机材料系气体阻透层可以列举以从硅、铝、镁和锌组成的一组中选择的1种或2种以上金属为主成分的金属氧化物、金属氮化物。这些是作为气体阻透性优异的材料已知的。这些氧化物层可以用溅射法、真空蒸气沉积法、离子镀法、等离子体CVD法等使材料从气相中堆积而形成膜的气相堆积法来制作。
其中,从气体阻透性、透明性、表面平滑性、挠曲性、膜应力、成本等观点来看,相对于硅原子数而言氧原子数的比例为1.5~2.0的硅氧化物为主成分的金属氧化物是良好的。
相对于硅氧化物的硅原子数而言氧原子数的比例,可以用X射线光电子分光法、X射线微分光法、俄歇电子分光法、卢瑟福反向散射法等分析确定。此比例小于1.5时挠曲性、透明性会下降,因而以1.5~2.0为适宜。
由金属氧化物组成的无机气体阻透层的厚度,以5~200nm范围为佳。比5nm薄时难以形成均匀的膜,会发生没有形成膜的部分,气体会从此部分渗透,使气体阻透性变差。而比200nm厚时,不仅透明性欠佳、挠曲性不良、也会发生龟裂,从而损害气体阻透性。又金属氧化物的特性会因制膜方法而异,但一般金属氧化物的膜厚增厚时金属氧化物层的残留应力会增大,因而本发明的透明导电性高分子基板在金属氧化物层形成后的卷曲增大而不好。进而,为获得高透明性,较好是相对于总重量而言含有5~30重量%氟化镁的上述硅氧化物。在这种情况下,从气体阻透性的观点来看,较好是厚度在60~200nm范围内。
这些气体阻透层既可以作为单独层使用,也可以多层并用。尤其在有机系气体阻透层与无机系气体阻透层并用的情况下,有机系气体阻透层对气体阻透层龟裂的优异耐性和无机系气体阻透层尤其对水蒸气的优异耐性会产生协同效果,因而是特别好的组合。进而,为增强设置气体阻透层的表面与气体阻透层的粘合性,也可以在这些层之间形成各种锚固层。这样的锚固层必须有耐药品性、透明性、及良好的层间粘合性,可以列举例如含硅树脂、环氧树脂等热固性树脂,紫外线固化性丙烯酸树脂等辐射固化性树脂,三聚氰胺树脂,聚氨酯树脂、醇酸树脂等。
设置了气体阻透层的层压薄膜的构成可以列举在本发明层压聚酯薄膜的涂布层上设置气体阻透层的构成、在基材薄膜上设置气体阻透层的构成、在涂布层与基材薄膜两者之上设置气体阻透层的构成。按照本发明,也提供这样的层压薄膜。
<透明导电层>
本发明层压聚酯薄膜之上也可以设置透明导电层而成为有用的层压薄膜。本发明层压聚酯薄膜用于电致发光(EL)、电子纸张、太阳能电池等用途上时必须有导电层。
导电层以透明性、导电性优异者为佳。这样的透明导电层可以列举添加了锡、碲、镉、钼、钨、氟作为杂质的氧化铟、氧化镉、氧化锡,添加了铝作为杂质的氧化锌、氧化钛等金属氧化膜。其中含有2~15重量%氧化锡的铟·锡氧化物(ITO)的薄膜因优异的导电性、透明性而较好。
上述透明导电层的膜厚可根据目标表面电阻设定。透明导电层的表面电阻值可因目的而异设定为300Ω/□~1Ω/□,其膜厚通常制作为10nm~400nm的范围。但在有可挠性的高分子基板上制作透明导电层时,从防止基板的弯曲应力引起的透明导电层破裂来看希望制作得薄一些,透明导电层的厚度以30nm~140nm为最好。又,为获得较低的电阻值,较好用130℃~200℃的温度进行热处理。
设置了透明导电层的层压薄膜的构成可以列举在本发明层压聚酯薄膜的涂层上设置透明导电层的构成、在基材薄膜上设置透明导电层的构成、在涂层与基材薄膜两者之上设置透明导电层的构成。
透明导电层既可经由硬涂层设置、也可经由气体阻透层设置、还可经由硬涂层及气体阻透层两者设置。按照本发明,也供这样的层压薄膜。
又,本发明中,作为依次经由气体阻透层及硬涂层而在涂层上设置了透明导电层的层压薄膜,每100μm膜厚的50%断裂能以在0.3J以上为宜、在0.4J以上更好、在0.5J以上最为适用。50%断裂能不足0.3J时耐冲击性不佳、容易发生裂痕,难以适用于可挠曲显示器的用途,因而不好。
<用途>
本发明的层压聚酯薄膜或层压薄膜可适用于显示器用途、太阳能电池用途、窗户张贴用途等。在显示器用途上,可适用于例如液晶、有机电致发光、电子纸张、触摸板、等离子体显示板(PDP)用的电磁波屏蔽薄膜等。
例如作为有机电致发光(EL)显示器使用时,可以在本发明的层压薄膜中层压发光材料。作为电子纸张使用时,可以在本发明的层压薄膜中层压影像显示元件。作为太阳能电池使用时,可以在本发明的层压薄膜中层压太阳能电池元件。在这些用途上使用本发明层压薄膜时,可以获得比其它材料更薄、而且耐冲击性更优异的物品。
作为电致发光(EL)材料,可以使用以下列举的色素系发光材料、金属络合物系发光材料、高分子系发光材料。
色素系发光材料,可以列举环戊二烯衍生物、四苯基丁二烯衍生物、三苯胺衍生物、二唑衍生物、吡唑并喹啉衍生物、二苯乙烯基苯衍生物、二苯乙烯基亚芳基衍生物、西洛卢(Sirole)衍生物、噻吩环化合物、吡啶环化合物、苝衍生物、苝酮衍生物、低聚噻吩衍生物、三富马尼胺衍生物、二唑二聚物、吡唑啉二聚物等。
又,金属络合物系发光材料可以列举铝喹啉酚络合物、苯并喹啉酚铍络合物、苯并唑锌络合物、苯并噻唑锌络合物、偶氮甲基锌络合物、卟啉锌络合物、铕络合物等中心金属为Al、Zn、Be等、或Tb、Eu、Dy等稀土金属、配体为二唑、噻二唑、苯基吡啶、苯基苯并咪唑、喹啉构造等的金属络合物等。
进而,高分子系发光材料可以列举聚对苯乙烯基衍生物、聚噻吩衍生物、聚对亚苯基衍生物、聚硅烷衍生物、聚乙炔衍生物、聚乙烯基咔唑、聚芴酮衍生物、聚芴衍生物、聚喹喔啉衍生物,及这些的共聚合体等。
附图简单说明
图1为用于50%断裂能测定的耐冲击性测定装置:图中序号如下。
1:砝码,300g或500g
2:U型冲击头,直径4mm,重142g
3:薄膜固定器
4:薄膜
〔实施例〕
以下列举实施例更详细地说明本发明。要说明的是,物性及特性是按以下列方法测定的。
(1)薄膜厚度
使用电子测微计(安立兹股分有限公司制,商品名为“K-312A型”)以针压30g测定薄膜的厚度。
(2)光雾度、全光线透射率
按照JIS规格K6714-1958,求得全光线透射率Tt(%)与散射光透射率Td(%),算出光雾度〔(Td/Tt)×100〕(%)。
(3)表面糙度
(3-1)三维中心线糙度SRa
使用非接触式三维糙度计(小坂研究所制,商品名为“ET30HK”),依下列条件测定表面糙度SRa。
波长780nm半导体激光
测定长1mm
采样间隔2μm
截断0.25mm
纵向(薄膜连续制膜方向)放大倍率十万倍,横向(与连续制膜方向垂直)放大倍率200倍,扫描线数100条
(3-2)十点平均糙度Rz
使用原子间力显微镜(Digital Instruments公司制,商品名为“NanoScope III AFM”J扫描器),依下列条件测定算出Rz。
探针:单结合硅传感器
扫描模式:分流模式
像素数:256×256数据点
扫描速度:2.0Hz
测定环境:室温,大气中
扫描范围:10μm□
(4)热收缩率
在薄膜样品上每隔30cm做一记号,在无荷重下在预定温度的炉中实施热处理,热处理后测定各记号的间隔距离;对于薄膜连续制膜方向(MD方向)与垂直于制膜方向的方向(TD方向),依下式算出其热收缩率。
热收缩率(%)=(热处理前记号间距离-热处理后记号间距离)
/热处理前记号间距离×100
(5)薄膜的折射率差指数Δn
使用棱镜耦合器(Metricon公司制,商品名为“Model 2010”),以波长473nm、633nm、830nm测定薄膜连续制膜方向和与制膜方向垂直的方向的折射率。将所得测定值代入下列Cauchy分散式。
ni=a+〔b/(λi)2〕+〔c/(λi)4〕
式中,λi为测定波长,ni为用波长λi测定的折射率。
解联立方程式,求出常数a,b,c。然后使用所得a,b,c的值,计算出波长589nm(Na,D线的波长)的折射率,以此作为薄膜的折射率。薄膜的折射率差指数Δn,可依下式算出。
Δn=(nTD-nMD)×1000
(6)涂层成分的折射率
高分子粘结剂以涂剂方式在90℃干燥成固体板状,以阿贝折射计(D线589nm)测定其折射率;而微粒是将90℃干固后的微粒悬浮于折射率不同的各种25℃液体中,以阿贝折射计(D线589nm)测定最透明悬浊液的折射率值。
(7)玻璃化温度
取试料约10毫克,封装于测定用铝制皿中,置于差示热量计(TAInstruments公司制,商品名为“DSC2920”)中,自25℃起以每分钟20℃的速度升温至300℃,在300℃保持5分钟后取出,直接入在冰上急冷;此皿再度置于差示热量计中,从-70℃起以每分钟10℃的速度升温,测定其玻璃化温度(Tg:℃)。
(8)特性粘度
特性粘度([η]dl/g),在35℃以邻-氯苯酚溶液测定。
(9)涂层厚度
将薄膜小片包埋于环氧树脂(Refinetec公司制,商品名为“EPOMOUNT”)中,使用Reichert-Jung公司制的Microtome 2050将包埋树脂切成各50nm厚薄片;用透射型电子显微镜(LEM-2000)以加速电压100KV、倍率10万倍观察,测定涂膜层的厚度。
(10)平均粒径
进行与涂层厚度测定相同的操作,测定100个微粒的粒径,以平均值作为平均粒径。
(11)杨氏模量
将薄膜样品切成宽10mm、长15cm的长条,以夹盘距离100mm、拉伸速度每分钟10mm、记录纸移动速度每分钟500mm用万能拉伸试验装置拉伸,从所得负荷-伸长曲线的上升部切线计算出薄膜连续制膜方向(MD方向)和与制膜方向垂直的方向(TD方向)的杨氏模量。
(12)滑动性
使用摩擦试验机(HOYO ERECTRONICS公司制,商品名“SET-1200S”),在切成10mm宽的薄膜上加40g/mm2的荷重T1(g),用外径6mm的不锈钢(SUS304)针(表面糙度Ra=20nm)以90度角接触的,测出以每秒20mm的速度通过时的卷取荷重T2(g),依下式算出摩擦系数μ,按下述基准评价。
μ=1n(T1/T2)
○:0.35以下的情况
△:0.35-0.40的情况
×:0.4以上的情况
(13)与硬涂层的粘合性
在聚酯薄膜的涂布面上形成厚度5μm的硬涂层,于硬涂层上实施棋盘目的交叉切割(1mm2目100个),其上以24mm宽的赛珞玢胶带(Nichiban公司制)粘贴;以180度剥离角度急速剥离后,观察其剥离面,按下述基准评价。
○:剥离面积低于10%,粘合力极好
△:剥离面积大于10%~低于40%,粘合力尚好
×:剥离面积大于40%,粘合力极不良
(14)耐冲击性
用图1的耐冲击性测定装置测定薄膜的50%断裂能E(J),依JIS规格K7211的标准算出。图1中的1为砝码(质量为300g或500g),2为U型冲击针(前端直径为4mm,质量142g),3为固定器,4为样品薄膜;依下式算出每100μm厚度的50%断裂能E50(J)。
E50=E×100(μm)/样品薄膜厚度(μm)
(15)涂层的组成
实施例与比较例使用的涂层的组成如表1所示。其中,构成此涂层的各成分如下。
表1
涂层的组成(重量%) | 高分子粘结剂的折射率 | ||||||
高分子粘结剂 | 微粒 | 其他 | |||||
聚酯树脂 | 丙烯酸树脂 | 微粒1 | 微粒2 | 蜡 | 湿润剂 | ||
涂液1 | 67 | 20 | 3 | - | 5 | 5 | 1.57 |
涂液2 | 67 | 20 | - | 3 | 5 | 5 | 1.57 |
涂液3 | 70 | 20 | - | - | 5 | 5 | 1.57 |
(聚酯)
由酸成分2,6-萘二羧酸63摩尔%间苯二甲酸32摩尔%/5-钠磺基间苯二甲酸5摩尔%,与二醇成分乙二醇90摩尔%/二甘醇10摩尔%所构成(Tg=76℃,平均分子量为12000)。要说明的是,聚酯是按照特开平06-116487号公报的实施例1记载的方法制造如下的。即,将2,6-萘二羧酸二甲酯42重量分、间苯二甲酸二甲酯17重量分、5-钠磺基间苯二甲酸二甲酯4重量分,乙二醇33重量份,二甘醇2重量分加入反应器中;再加入四丁氧基钛0.05重量分,于氮气氛围下加热并将温度控制在230℃,将生成的甲醇蒸出,进行酯交换反应。其次使反应系的温度徐徐升至255℃,系内维持在1mmHg的减压,进行缩聚反应,即得聚酯。
(丙烯酸树脂)
由甲基丙烯酸甲酯30摩尔%/2-异丙烯基-2-唑啉30摩尔%/聚环氧乙烷(n=10)甲基丙烯酸酯10摩尔%/丙烯酸酰胺30摩尔%所构成(Tg=50℃)。要说明的是,丙烯酸树脂是按照特开昭63-37167号公报的制造例1~3记载的方法制造如下。即,在四口烧瓶中加入离子交换水302重量分,于氮气流中加热至60℃;其次加入聚合引发剂过硫酸铵0.5重量分,亚硝酸氢钠0.2重量分,进而用3小时时间滴加单体类甲基丙烯酸甲酯23.3重量分、2-异丙烯基-2-唑啉22.6重量份、聚环氧乙烷(n=10)甲基丙烯酸酯40.7重量分、丙烯酸酰胺13.3重量分的混合物,边滴加边调整,使得液温保持在60~70℃之间。滴加完毕后也在同温度范围保持2小时,继续在搅拌下反应;然后冷却,得到固形分为25重量%的丙烯酸树脂水分散体。
(微粒1)
使用二氧化硅及二氧化钛的复合无机微粒(平均粒径100nm)。要说明的是,微米1是按照特开平7-2520号公报的制造例及实施例记载的方法制造如下的。在带有搅拌桨的内容积4升玻璃制反应容器中加入甲醇140g、异丙醇260g、及氨水(25重量%)100g,配制成反应液,使反应液温度保持在40℃继续搅拌。其次,在3升三角烧瓶中,加入四甲氧基硅〔Si(OMe)4,Colcoat公司供应,商品名“METHYLSILICATE 39”〕542g,边搅拌边加入甲醇195g及0.1重量%盐酸水溶液(和光纯药工业股份有限公司制35重量%盐酸以水稀释1000倍)28g,搅拌约10分钟。随后加入四异丙氧基钛〔Ti(O-i-Pr)4,日本曹达股份有限公司制,商品名为“A-1(TPT)”〕300g以异丙醇634g稀释的液体,得到透明均匀溶液(四烷氧基硅与四烷氧基钛的共缩合物)。将上述均匀溶液1699g及氨水(25重量%)480g分别滴加到上述反应液中,最初使滴加速度减慢,终盘时徐徐加大速度,使得能以2小时同时滴加完毕。滴加结束后将所得共水解物过滤,在50℃使有机溶剂干燥,然后分散于水中,得到浓度10重量%。折射率1.56的微粒1。
(微粒2)
使用二氧化硅填充剂(平均粒径200nm,折射率1.42)(日产化学股份有限公司制,商品名为“MP-2040”)。
(蜡)
使用巴西棕榈蜡(中京油脂股份有限公司制,商品名为“SELOSOL524”)。
(湿润剂)
使用聚氧乙烯(n=7)月桂基醚(三洋化成股份有限公司制,商品名为“NAROACTY-N-70”)。
〔实施例1〕
使用2,6-萘二羧酸二甲酯100重量分,及乙二醇60重量分,与酯交换催化剂乙酸锰四水合物0.03重量分,边从150℃徐徐升温至238℃边进行120分钟酯交换反应;其间反应温度达到170℃时添加三氧化锑0.024重量分,酯交换反应完了后加入磷酸三甲酯(在乙二醇中在135℃、5小时、0.11~0.16MPa加压下的加热处理溶液:磷酸三甲酯换算量0.023重量分);然后将反应生成物移至聚合反应器中,升温至290℃,在低于27Pa的高真空下进行缩聚反应,得到特性粘度0.61dl/g、实质上不含微粒的聚-2,6-萘二羧酸乙二醇酯。
此聚-2,6-萘二羧酸乙二醇酯的切片在170℃下干燥6小时后供给挤塑机漏斗,于305℃熔融温度下熔融,用平均筛目17μm的不锈钢细丝滤网过滤,经3mm缝隙状模头挤出到表面温度60℃的旋转冷却鼓上,急速冷却,得到未拉伸薄膜。这样得到的未拉伸薄膜在120℃预热,进而在低速、高速辊之间从15mm上方用900℃IR加热器加热,使得在纵向上拉伸3.1倍。这种纵拉伸后的薄膜的一面上用辊涂器涂布表1的涂液1,使得干燥后涂膜厚度达到0.1μm左右。
随后供给展幅机,于145℃在横向上拉伸3.2倍。所得的双轴取向薄膜在240℃温度热定形40秒钟,得到厚度200μm的层压聚酯薄膜。所得薄膜的特性如表2所示。可获得厚度较薄、耐冲击性优异、而且滑动性、透明性、尺寸稳定性、粘合性均优异的薄膜。
〔实施例2〕
实施例1得到的层压聚酯薄膜用辊筒卷取后,用IR加热器的加热区域,以处理温度220℃、松弛率0.5%进行松弛处理,得到双轴取向薄膜。所得薄膜的特性如表2所示。可获得厚度较薄、耐冲击性优异、而且滑动性、透明性、尺寸稳定性、粘合性均优异的薄膜。其中尺寸稳定性特优。
表2
实施例1 | 实施例2 | ||||
制膜条件 | 厚度 | μm | 200 | ||
拉伸倍率(纵×横) | 倍 | 3.1×3.2 | |||
评价项目 | 光雾度 | % | 1.0 | 1.0 | |
全光线透射率 | % | 87 | 87 | ||
中心线表面糙度 | SRa | nm | 11 | 11 | |
10点平均糙度 | Rz | nm | 100 | 100 | |
热收缩率(230℃×30分钟) | MD方向 | % | 3.0 | 0.5 | |
TD方向 | % | 4.0 | 0.5 | ||
折射率差指数 | Δn | -1 | 3 | ||
杨氏模量 | MD方向 | GPa | 5.8 | 5.6 | |
TD方向 | GPa | 5.8 | 5.6 | ||
滑动性 | ○ | ○ | |||
硬涂层粘合性 | ○ | ○ | |||
50%断裂能(E50) | J | 0.6 | 0.6 | ||
综合评价 | ○ | ◎ |
〔比较例1〕
除实施例1使用的聚-2,6-萘二羧酸乙二醇酯中加入平均粒径0.35μm的球状二氧化硅微粒0.1重量%混练制作、以拉伸倍率为纵向3.7倍、横向4.0倍进行拉伸、薄膜厚度为75μm外,用和实施例1相同的方法得到双轴拉伸薄膜。所得薄膜的特性如表3所示。所得薄膜因含滑动剂之故,光雾度较高,全光线透射率也差,变成不透明薄膜。又,由于拉伸倍率大而变成热收缩率大的薄膜。
〔比较例2〕
除实施例1中涂层使用的涂液1换为涂液2外同实施例1一样进行,得到双轴拉伸薄膜。所得薄膜的特性如表3所示。所得薄膜由于涂层的微粒与高分子粘结剂的折射率差较大而变成光雾度高的不透明薄膜。
〔比较例3〕
除实施例1中涂层使用的涂液1换为涂液3外同实施例1一样进行,得到双轴拉伸薄膜。所得薄膜的特性如表3所示。所得薄膜由于涂层中没有微粒存在而变成滑动性不良的薄膜。
表3
比较例1 | 比较例2 | 比较例3 | ||||
制膜条件 | 厚度 | μm | 75 | 200 | ||
拉伸倍率(纵×横) | 倍 | 3.7×4.0 | 3.1×3.2 | |||
评价项目 | 光雾度 | % | 21.0 | 1.7 | 0.8 | |
全光线透射率 | % | 82 | 87 | 87 | ||
中心线表面糙度 | SRa | nm | 21 | 33 | 3 | |
10点平均糙度 | Rz | nm | 70 | 160 | 33 | |
热收缩率(230℃×30分钟) | MD方向 | % | 4.2 | 3.0 | 3.0 | |
TD方向 | % | 4.7 | 4.0 | 4.0 | ||
折射率差指数 | Δn | -16 | -1 | -1 | ||
杨氏模量 | MD方向 | GPa | 6.1 | 5.8 | 5.8 | |
TD方向 | GPa | 6.4 | 5.8 | 5.8 | ||
滑动性 | ○ | ○ | × | |||
硬涂层粘合性 | × | ○ | ○ | |||
50%断裂能(E50) | J | 0.6 | 0.6 | 0.6 | ||
综合评价 | × | × | × |
〔比较例4〕
除没有涂层、拉伸倍率如表4所示那样变更外,同实施例1一样进行,得到双轴拉伸薄膜。所得薄膜的特性如表4所示。所得薄膜由于没有涂层之故,其滑动性、对硬涂层的粘合性均不良;且变成各向异性大的薄膜。
〔比较例5〕
将对苯二甲酸甲酯96重量分、乙二醇58重量分、乙酸锰0.038重量分及三氧化锑0.041重量分分别加入反应器中,边在搅拌下蒸出甲醇直至内温达到240℃边进行酯交换反应;该酯交换反应结束后加入磷酸三甲酯0.097重量分。随后使反应生成物升温,最终在280℃在高真空条件下进行缩聚反应。得到特性粘度([η])0.64的聚对苯二甲酸乙二醇酯切片。
其次,将此聚对苯二甲酸乙二醇酯切片在170℃干燥3小时后,供给双螺杆挤塑机于280℃熔融混练、急冷固化,得到母练胶切片。
此聚对苯二甲酸乙二醇酯粒料在160℃干燥3小时后,供给挤塑机漏斗,在熔融温度295℃熔融,用保持在20℃的冷却鼓急冷固化,得到未延伸薄膜。该未延伸薄膜于95℃以3.5倍进行纵向拉伸;然后在下面、进而在上面涂布下述涂剂,使其干燥后的厚度达到0.1μm;在110℃以3.8倍进行横向拉伸后于230℃进行热处理,得到厚度100μm的双轴拉伸薄膜。所得薄膜的特性如表4所示。虽然光雾度、全光线透射率良好,但成为热收缩率大、尺寸稳定性不佳的薄膜。
〔比较例6〕
评价了市售厚度200μm的聚醚砜薄膜(住友Bakelite公司制,商品名为“FS-1300”)。评估结果如表4所示。虽然光雾度、全光线透射率、热收缩率良好,但是滑动困难、耐冲击性也不佳的薄膜。
表4
比较例4 | 比较例5 | 比较例6 | ||||
制膜条件 | 厚度 | μm | 75 | 100 | 200 | |
拉伸倍率(纵×横) | 倍 | 4.0×3.3 | 3.5×3.8 | - | ||
评价项目 | 光雾度 | % | 0.7 | 0.8 | 0.7 | |
全光线透射率 | % | 85 | 90 | 88 | ||
中心线表面糙度 | SRa | nm | 3 | 11 | 5 | |
10点平均糙度 | Rz | nm | 15 | 100 | 12 | |
热收缩率(230℃×30分钟) | MD方向 | % | 2.0 | 6.8 | 0.1 | |
TD方向 | % | 0.4 | 3.4 | 0.6 | ||
折射率差指数 | Δn | 65 | 12 | 1 | ||
杨氏模量 | MD方向 | GPa | 6.7 | 5.1 | 2.3 | |
TD方向 | GPa | 5.7 | 5.7 | 2.3 | ||
滑动性 | × | ○ | × | |||
硬涂层粘合性 | × | ○ | ○ | |||
50%断裂能(E50) | J | 0.6 | 0.4 | 0.2 | ||
综合评价 | × | × | △ |
〔实施例3〕
在实施例1所得薄膜的涂层侧用辊涂法涂布用来形成硬涂层的硬涂层剂(大日精化工业股份有限公司制,商品名为“PETD-31”)与1-羟基环苯基酮一起搅拌脱泡后的涂布剂,使其干燥后厚度可达5μm程度,干燥后以电子束在175kV及10Mrad的条件下照射,形成硬涂膜;进而在硬涂层反面使用真空蒸气沉积装置以电子束加热使由硅与二氧化硅的混合物组成的蒸气沉积材料蒸发,形成厚度20nm的SiOx膜。
其次,在溅射装置中导入Ar·O2混合气(O2浓度为1.4容积%),调整到压力为0.27Pa,使用ITO靶(SnO2浓度为5重量%),在输入功率密度为1w/cm2的条件下进行DC溅射,层压厚度达130μm后,在150℃进行2小时热处理,得由ITO膜组成的层压薄膜。所得薄膜的特性如表5所示。可获得构成体薄、耐冲击性优异的物品。
〔实施例4〕
在实施例2所得薄膜上用与实施例3相同的方法,得到层压了硬涂层、气体阻透层、透明导电层的薄膜。所得薄膜的特性如表5所示。可获得构成体薄、耐冲击性优异的物品。
〔比较例7〕
在实施例6所得薄膜上用与实施例3相同的方法,得到层压了硬涂层、气体阻透层、透明导电层的薄膜。所得薄膜的特性如表5所示。成为耐冲击性不良、容易破裂的层压薄膜。
〔比较例8〕
从市售的带有ITO膜的玻璃(Corning公司制,商品名为“#1737”)所得特性如表5所示;是耐冲击性非常不良者。
表5
实施例3 | 实施例4 | 比较例7 | 比较例8 | ||
50%断裂能(E50) | J | 0.6 | 0.6 | 0.2 | 0.01 |
按照本发明,可以提供滑动性、透明性、尺寸稳定性、耐冲击性,粘合性均优异的层压聚酯薄膜。
Claims (17)
1.一种层压聚酯薄膜,包含由聚-2,6-萘二羧酸乙二醇酯构成、在至少一个方向上拉伸的基材薄膜、和在该基材薄膜至少一面上设置的涂层,其特征在于所述涂层含有高分子粘结剂与微粒,该微粒的折射率与高分子粘结剂的折射率实质上相同,均为1.50~1.60,而且层压聚酯薄膜的光雾度在1.5%或以下、全光线透射率在85%或以上、每100μm薄膜厚度的50%断裂能在0.3J或以上、在230℃30分钟条件下的热收缩率在4%或以下。
2.按照权利要求1的层压聚酯薄膜,其中在230℃30分钟条件下的热收缩率在1%或以下。
3.按照权利要求1的层压聚酯薄膜,其中高分子粘结剂是聚酯树脂和含有唑啉基与聚烯化氧基的丙烯酸树脂的混合物。
4.按照权利要求1的层压聚酯薄膜,其中两个表面的三维中心线平均糙度SRa均为2~20nm且至少一面的十点平均糙度Rz为50~150nm。
5.按照权利要求1的层压聚酯薄膜,其中基材薄膜是以连续制膜法制膜的,当连续制膜方向的折射率为nMD、与连续制膜方向垂直的方向的折射率为nTD时,下式所示的薄膜面方向的折射率差指数Δn的绝对值为50或以下,Δn=(nMD-nTD)×1000。
6.按照权利要求1的层压聚酯薄膜,其中杨氏模量为3~15GPa。
7.一种层压薄膜,其特征在于在权利要求1的层压聚酯薄膜的涂层上设置硬涂层。
8.一种层压薄膜,其特征在于在权利要求7的层压薄膜的硬涂层上设置气体阻透层。
9.一种层压薄膜,其特征在于在权利要求8的层压薄膜的气体阻透层上设置透明导电层。
10.一种层压薄膜,其特征在于在权利要求8的层压薄膜的气体阻透层设置面的反面上设置透明导电层。
11.按照权利要求9的层压薄膜,其中每100μm薄膜厚度的50%断裂能在0.3J或以上。
12.按照权利要求1的层压聚酯薄膜,作为电致发光用基板薄膜使用。
13.按照权利要求11的层压薄膜,作为电致发光用基板薄膜使用。
14.按照权利要求1的层压聚酯薄膜,作为电子纸张用基板薄膜使用。
15.按照权利要求11的层压薄膜,作为电子纸张用基板薄膜使用。
16.按照权利要求1的层压聚酯薄膜,作为太阳能电池用基板薄膜使用。
17.按照权利要求11的层压薄膜,作为太阳能电池用基板薄膜使用。
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CN104342049B (zh) * | 2013-07-31 | 2019-07-23 | 日东电工株式会社 | 粘合片以及光学构件 |
CN107851485A (zh) * | 2015-07-23 | 2018-03-27 | 富士胶片株式会社 | 层叠体 |
Also Published As
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EP1510540A1 (en) | 2005-03-02 |
TW200307602A (en) | 2003-12-16 |
CN1659216A (zh) | 2005-08-24 |
TWI289507B (en) | 2007-11-11 |
DE60321678D1 (de) | 2008-07-31 |
KR100974841B1 (ko) | 2010-08-11 |
JP4052021B2 (ja) | 2008-02-27 |
KR20050004779A (ko) | 2005-01-12 |
AU2003241732A1 (en) | 2003-12-19 |
JP2004009362A (ja) | 2004-01-15 |
WO2003102057A1 (fr) | 2003-12-11 |
US20040265539A1 (en) | 2004-12-30 |
EP1510540B1 (en) | 2008-06-18 |
EP1510540A4 (en) | 2005-07-20 |
US7022388B2 (en) | 2006-04-04 |
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