CN105683286A - 阻燃性双轴取向聚酯膜、由其形成的阻燃性聚酯膜层合体和柔性电路基板 - Google Patents
阻燃性双轴取向聚酯膜、由其形成的阻燃性聚酯膜层合体和柔性电路基板 Download PDFInfo
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- CN105683286A CN105683286A CN201480059439.XA CN201480059439A CN105683286A CN 105683286 A CN105683286 A CN 105683286A CN 201480059439 A CN201480059439 A CN 201480059439A CN 105683286 A CN105683286 A CN 105683286A
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- polyester film
- retardant
- film
- flame
- weight
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Classifications
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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
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- 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
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/09—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyesters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本发明的目的在于提供聚酯膜本身用磷类阻燃剂阻燃、这些阻燃剂导致的聚酯膜的耐水解性的降低得到抑制、且阻燃剂导致的制膜性降低和机械特性的降低得到抑制的阻燃性双轴取向聚酯膜,由其形成的阻燃性聚酯膜层合体以及柔性电路基板。本发明通过阻燃性双轴取向聚酯膜获得,其中,以聚酯膜重量为基准,含有70重量%以上99.5重量%以下的聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯,以及0.5重量%以上30重量%以下的以特定的次膦酸盐或双次膦酸盐表示的平均粒径0.5-3.0μm的阻燃剂颗粒,且该聚酯膜中所含的最大长度10μm以上的粗大颗粒的个数为10个/m2以下。
Description
技术领域
本发明涉及具有阻燃性的双轴取向聚酯膜、由其形成的阻燃性聚酯膜层合体和柔性电路基板,更具体地说,涉及阻燃性优异、同时制膜性降低和机械特性降低得到抑制的阻燃性双轴取向聚酯膜,由其形成的阻燃性聚酯膜层合体和柔性电路基板。
背景技术
随着便携电话等电子设备的技术进步,柔性印刷电路(以下可简称为FPC)基板的需求急速发展。近年来,随着制造物责任法的实施,为了确保对火灾的安全性,人们要求FPC所使用的树脂的阻燃化。
虽然以往所使用的有机卤素化合物、含卤素有机磷化合物等卤素类阻燃剂的阻燃效果高,但是在成型·加工时卤素游离,生成腐蚀性的卤化氢气体,被指出腐蚀成型·加工机器的可能性,以及使作业环境恶化的可能性。还被指出这些卤素类阻燃剂在火灾等燃烧时产生卤化氢等气体的可能性。因此,近年来人们希望使用不含有卤素的阻燃剂以代替卤素类阻燃剂。
使用聚酯膜、特别是聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯的双轴拉伸膜具有优异的机械性质、耐热性、耐化学药品性,因此作为磁带、照相软片、包装用膜、电子部件用膜、电绝缘膜、金属层合用膜和保护用膜等的原材料广泛应用。
作为聚酯树脂的阻燃化方法之一,人们探讨了将磷化合物与聚酯共聚的方法。例如日本特开2007-9111号公报(专利文献1)中公开:通过在羧基次膦酸成分中使用特定的羧基次膦酸成分,即使不与其它磷化合物并用,也可以以少量对聚2,6-萘二甲酸乙二醇酯赋予高阻燃性。但是,如专利文献1那样含有羧基次膦酸化合物的聚2,6-萘二甲酸乙二醇酯膜虽然在膜状态下表现高阻燃性,但是对于加工成柔性印刷电路等用途后的阻燃性,则膜的阻燃性可能无法再现。
作为其它磷类阻燃剂,例如在日本特开2009-179037号公报(专利文献2)、日本特开2010-89334号公报(专利文献3)中提出:将含有次膦酸金属盐等无机金属的磷酸类衍生物的阻燃层与聚酯膜层合而成的层合膜。但是所提出的层合膜是鉴于多孔基材膜的膜内部的孔洞结构导致燃烧性高,而在基材膜上设置使用阻燃剂和固化剂的阻燃层的技术。另外日本特开2010-229390号公报(专利文献4)中记载了配合有无机金属的磷酸类衍生物的组合物和阻燃被覆电线,但这是使热塑性弹性体树脂阻燃化的技术,热塑性弹性体树脂是伸长率高的树脂,因此不太会发生随着阻燃剂的添加而物性降低的问题。另外国际公开第2012/090732号小册子(专利文献5)中提出了含有次膦酸盐(phosphinate)或双次膦酸盐(diphosphinate)的阻燃性聚酯膜,并提出了将聚对苯二甲酸亚烷基酯或聚萘二甲酸亚烷基酯这样的聚酯膜本身用磷类阻燃剂进行阻燃化,并且这些阻燃剂导致的耐水解性降低得到抑制的阻燃性双轴取向聚酯膜。
专利文献1:日本特开2007-9111号公报
专利文献2:日本特开2009-179037号公报
专利文献3:日本特开2010-89334号公报
专利文献4:日本特开2010-229390号公报
专利文献5:国际公开第2012/090732号小册子。
发明内容
发明所要解决的课题
本发明人在推进使用次膦酸盐或双次膦酸盐作为阻燃剂的聚酯膜的研究的过程中发现,在将这些阻燃剂添加到聚酯膜时,容易伴有制膜性降低以及所得膜的机械强度容易降低的新课题。
即,本发明的目的在于消除所述课题,提供:将聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯这样的聚酯膜本身用磷类阻燃剂阻燃化、这些阻燃剂导致的耐水解性降低得到抑制、并且阻燃剂导致的制膜性降低和机械特性降低也得到抑制的阻燃性双轴取向聚酯膜,以及由其形成的阻燃性聚酯膜层合体和柔性电路基板。
解决课题的方案
本发明人为解决前述课题进行了深入的研究,结果发现:次膦酸盐或双次膦酸盐不与聚酯相容,在膜中以如颗粒等那样的杂质形式存在,并且粗大颗粒的存在比例高,因此由于这些因素引起制膜性降低和机械特性降低,还发现:通过在控制粒径的同时控制阻燃剂的粗大颗粒的频率,制膜性和机械强度提高,从而完成了本发明。
即,本发明的目的通过阻燃性双轴取向聚酯膜(项目1)实现,所述双轴取向聚酯膜以聚酯膜重量为基准,含有70重量%以上99.5重量%以下的聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯、以及0.5重量%以上30重量%以下的下式(1)或下式(2)所示的平均粒径0.5-3.0μm的阻燃剂颗粒,且该聚酯膜中所含的最大长度10μm以上的粗大颗粒的个数为10个/m2以下,
[化1]
(式中,R1、R2为氢、碳原子数1-6的烷基和/或芳基,M表示金属,m表示M的价数)
[化2]
(式中,R3、R4为氢、碳原子数1-6的烷基和/或芳基,R5为碳原子数1-6的亚烷基或碳原子数6-10的亚芳基、烷基亚芳基或芳基亚烷基,M表示金属,n表示M的价数)。
本发明的阻燃性双轴取向聚酯膜也优选包含以下方案。
(项目2)项目1所述的阻燃性双轴取向聚酯膜,其中,所述聚酯膜的机械强度为150MPa以上。
(项目3)项目1或2所述的阻燃性双轴取向聚酯膜,其中,在121℃、2个气压的饱和水蒸汽中处理10小时后,所述聚酯膜的拉伸强度保持率为80%以上。
(项目4)项目1-3中任一项所述的阻燃性双轴取向聚酯膜,其中,所述聚酯膜的表面粗糙度Ra为0.1μm以上且低于0.5μm。
本发明也包含以下方案的发明。
(项目5)阻燃性聚酯膜层合体,该层合体是项目1-4中任一项所述的阻燃性双轴取向聚酯膜与金属层层合而成。
(项目6)项目5所述的阻燃性聚酯膜层合体,该层合体用于柔性印刷电路基板用。
(项目7)柔性电路基板,该柔性电路基板使用项目5或6所述的阻燃性聚酯膜层合体。
发明效果
根据本发明,本发明的阻燃性双轴取向聚酯膜的制膜性优异,不会使聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯这样的聚酯所具有的机械特性、耐水解性降低,具备高阻燃性,因此可适宜地用于例如柔性印刷电路基板、扁平电缆、太阳能电池用背板等。
具体实施方式
以下详细说明本发明。
<阻燃性双轴取向聚酯膜>
本发明的阻燃性双轴取向聚酯膜中,以聚酯膜重量为基准,以70重量%以上99.5重量%以下的范围含有聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯作为聚合物成分,还以0.5重量%以上30重量%以下的范围含有下式(1)或下式(2)所示的平均粒径0.5-3.0μm的阻燃剂颗粒,且该聚酯膜中所含的最大长度10μm以上的粗大颗粒的个数为10个/m2以下,
[化3]
(式中,R1、R2为氢、碳原子数1-6的烷基和/或芳基,M表示金属,m表示M的价数),
[化4]
(式中,R3、R4为氢、碳原子数1-6的烷基和/或芳基,R5为碳原子数1-6的亚烷基或碳原子数6-10的亚芳基、烷基亚芳基或芳基亚烷基,M表示金属,n表示M的价数)。
(聚酯)
本发明的阻燃性双轴取向聚酯膜使用聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯作为聚合物成分。该聚合物成分的含量是以聚酯膜重量为基准,为70重量%以上99.5重量%以下的范围。这些聚合物成分的含量的下限值优选为75重量%,更优选为78重量%,进一步优选为80重量%,特别优选为85重量%。
这些聚合物成分的含量的上限值,由于与后述的阻燃成分的含量的关系,优选为99重量%,更优选96重量%,进一步优选92重量%,特别优选90重量%。
这些聚合物成分的含量若低于下限值,则膜的机械强度降低。另一方面,这些聚合物成分的含量若超过上限值,则阻燃成分的含量相对少,无法表现充分的阻燃性。
本发明的聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯在不损害本发明的目的的范围内可以是具有主成分以外的成分(以下可称为共聚成分)的共聚物,以这些聚酯的全部重复单元的摩尔数为基准,可优选在低于25摩尔%的范围内使用共聚成分,更优选为20摩尔%以下,进一步优选15摩尔%以下。
所述共聚成分例如可例举:草酸、己二酸、邻苯二甲酸、癸二酸、十二烷二甲酸、间苯二甲酸、对苯二甲酸、1,4-环己烷二甲酸、4,4’-二苯基二甲酸、苯基茚满二甲酸、2,6-萘二甲酸、2,7-萘二甲酸、萘满二甲酸、萘烷二甲酸、二苯基醚二甲酸等二羧酸,对羟基苯甲酸、对羟乙氧基苯甲酸等羟基羧酸,或乙二醇、三亚甲基二醇、四亚甲基二醇、六亚甲基二醇、环己烷二甲醇、新戊二醇、双酚S(bisphenolsulfone)的环氧乙烷加成产物、双酚A的环氧乙烷加成产物、二甘醇、聚氧化乙烯二醇等二醇,其中可优选使用主成分以外的成分。这些共聚成分可以使用1种或2种以上。
这些共聚成分可以作为单体成分配合、共聚,还可以通过与其它聚酯的酯交换反应共聚。
本发明的聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯在不损害本发明的目的的范围内可以是至少2种聚酯的掺混物,或与聚酯以外的热塑性树脂的掺混物。这些其它成分可以以聚酯膜的重量为基准、在20重量%以下的范围内使用,更优选为15重量%以下,进一步优选10重量%以下。聚酯以外的热塑性树脂例如可例举:聚烯烃类树脂、聚苯乙烯类树脂、聚酰亚胺类树脂等。
作为这些聚酯的特性粘度,以邻氯苯酚为溶剂、在25℃下测定的特性粘度优选为0.4dl/g以上1.5dl/g以下,进一步优选为0.5dl/g以上1.2dl/g以下。
(阻燃成分)
本发明中,作为阻燃成分,以阻燃剂颗粒的形式使用下式(1)所示的次膦酸盐或下式(2)所示的双次膦酸盐。以下将它们总括称为次膦酸盐类。
[化5]
(式中,R1、R2为氢、碳原子数1-6的烷基和/或芳基,M表示金属,m表示M的价数)
[化6]
(式中,R3、R4为氢、碳原子数1-6的烷基和/或芳基,R5为碳原子数1-6的亚烷基或碳原子数6-10的亚芳基、烷基亚芳基或芳基亚烷基,M表示金属,n表示M的价数)。
所述次膦酸盐是也被称为次膦酸金属盐的化合物,R1、R2可例举氢、甲基、乙基、正丙基、异丙基、正丁基、叔丁基、戊基、己基、苯基。M可例举:铝、镁、钙,价数m为2-4的整数。具体来说,可举出:二甲基次膦酸钙、甲基乙基次膦酸钙、二乙基次膦酸钙、苯基次膦酸钙、联苯次膦酸钙、二甲基次膦酸镁、甲基乙基次膦酸镁、二乙基次膦酸镁、苯基次膦酸镁、联苯次膦酸镁、二甲基次膦酸铝、甲基乙基次膦酸铝、二乙基次膦酸铝、苯基次膦酸铝、联苯次膦酸铝。
双次膦酸盐中,R3、R4可例举:氢、甲基、乙基、正丙基、异丙基、正丁基、叔丁基、戊基、己基、苯基,R5可例举:亚甲基、亚乙基、亚丙基、亚丁基、亚戊基、亚己基、亚苯基。M可例举:铝、镁、钙,价数n为2-4的整数。
式(2)所示的双次膦酸盐可举出:乙烷-1,2-双次膦酸钙等的链烷双次膦酸钙,乙烷-1,2-双(甲基次膦酸)钙等的链烷双(烷基次膦酸)钙,链烷双次膦酸镁、链烷双(烷基次膦酸)镁、链烷双次膦酸铝、链烷双(烷基次膦酸)铝等。
这些次膦酸盐类中,特别优选二乙基次膦酸铝。
本发明通过使用所述次膦酸盐类作为阻燃成分,与以往的磷类阻燃剂相比,对聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯这样的强度高的聚酯的物性降低的影响少,可以添加大量的阻燃成分到迄今无法添加的程度。因此例如加工为与金属层层合使用的用途时,以往的话是金属层合体的阻燃性与层合金属层之前的阻燃性聚酯膜相比降低,与此相对,本发明具有可获得与阻燃性聚酯膜本身同样的高阻燃性的特征。
所述次膦酸盐类的含量是以聚酯膜的重量为基准,为0.5重量%以上30重量%以下。所述次膦酸盐类的含量的下限值优选为1重量%,更优选4重量%,进一步优选8重量%,特别优选10重量%。该次膦酸盐类的含量的上限值优选为25重量%,更优选22重量%,进一步优选20重量%,特别优选15重量%。次膦酸盐类的含量若低于下限值,则阻燃性不充分,而次膦酸盐类的含量若超过上限值,则膜制膜性和机械强度降低。
所述次膦酸盐类具有颗粒形状,本发明中称为阻燃剂颗粒。本发明的阻燃剂颗粒的平均粒径为0.5μm以上3.0μm以下,该平均粒径的下限优选为1.0μm,进一步优选1.5μm。该阻燃剂颗粒的平均粒径的上限优选为2.5μm。平均粒径若低于下限,则可能膜制膜时的操作性降低,或膜中的分散性不充分。而若为超过上限的平均粒径,则可能膜制膜时容易断裂,制膜性降低,或者即使可以制膜,膜的强度也降低。
本发明的阻燃性双轴取向聚酯膜中所含的最大长度10μm以上的粗大颗粒的个数要求为10个/m2以下,进一步优选为5个/m2以下。认识到:所述阻燃剂颗粒的粒径的分布非常广泛,这些粗大颗粒对于制膜性降低、膜强度降低有影响。即认识到:所述阻燃剂颗粒的粒径分布与聚酯膜中通用的颗粒的粒径分布相比,分布范围非常广,因此,在添加阻燃剂颗粒之前不进行前处理时,超过上述范围数目的粗大颗粒存在于膜中,因此引起制膜性、膜强度的降低。
为了使粗大颗粒的个数为上述范围,例如可在制膜工序之前进行将阻燃剂颗粒粉碎、分级等加工,预先除去这些粗大颗粒,由此获得高机械强度和优异外观性的阻燃性双轴取向聚酯膜。
这里,阻燃剂颗粒的平均粒径如测定方法一栏所说明的,对于聚酯膜的截面,使用HIROXCo.,Ltd.(株式会社ハイロックス)数字显微镜KH-3000,以3500倍的倍率取样20个颗粒,测定各粒径中的最大长度,从20点中除去最小值和最大值,由18点的平均值求出。
粗大颗粒的最大长度可以使用万能投影仪,通过透射照明放大至20倍来测定颗粒的最大长度而求出。
(磷原子浓度)
本发明中的磷原子浓度是以聚酯膜的重量为基准,优选为0.1重量%以上7重量%以下。所述磷原子浓度的下限值更优选为1.0重量%,进一步优选2.0重量%,特别优选2.5重量%。而所述磷原子浓度的上限值更优选为6.0重量%,进一步优选5.0重量%。
本发明中,通过对聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯这样的强度高的聚酯使用本发明的由次膦酸盐类形成的特定尺寸的阻燃剂颗粒,与以往的添加型磷类成分或共聚型磷类成分相比,在无损聚酯的机械特性方面具有特征。
另一方面,若将磷原子浓度提高至超过上限值,则所添加的次膦酸盐类的量过多,膜的机械强度和制膜性欠缺。在接近于磷原子浓度的下限值的范围、即,在与以往的磷类成分含量接近的范围内,也具有如下特征:与其它磷类成分相比可表现高阻燃性,并在加工为与金属层层合使用的用途时也可以再现与阻燃性聚酯膜本身同样高的阻燃性。即使在磷类成分的含量少的范围也可以表现所述效果的原因被认为是由于构成次膦酸盐类的金属成分带来的自由基捕获效果。
(其它添加剂)
本发明的阻燃性双轴取向聚酯膜中,为了提高膜的操作性,在不损害发明效果的范围内可以添加惰性颗粒等。所述惰性颗粒例如可举出含有元素周期表中第IIA、第IIB、第IVA、第IVB族元素的无机颗粒(例如高岭土、氧化铝、氧化钛、碳酸钙、二氧化硅等),交联有机硅树脂、交联聚苯乙烯、交联丙烯酸树脂颗粒等由耐热性高的聚合物形成的颗粒。
在使膜中含有惰性颗粒时,惰性颗粒的平均粒径优选0.001-5μm的范围,以聚酯膜重量为基准,优选在0.01-10重量%的范围含有,进一步优选为0.05-5重量%,特别优选0.05-3重量%。
本发明的阻燃性双轴取向聚酯膜中可以进一步根据需要、在不损害本发明的目的的范围内配合热稳定剂、抗氧化剂、紫外线吸收剂、脱模剂、着色剂、抗静电剂等添加剂。
(膜厚度)
本发明的聚酯膜的厚度优选为2μm以上200μm以下。以往,若通过在聚酯膜中添加磷类阻燃剂的方法使其阻燃化,则引起聚酯膜的机械特性、耐水解性降低,因此并不是将聚酯膜本身用磷类阻燃剂阻燃化,而是采取将含有阻燃剂的其它层与聚酯膜层合的方法,与此相对,本发明具有可对具有所述厚度的聚酯膜本身添加磷类阻燃剂的特征。
聚酯膜的厚度可根据用途在上述范围内调节。例如为扁平电缆用途时,更优选为2-100μm,进一步优选5-75μm,特别优选10-50μm。为柔性印刷电路基板用途时,更优选为2-150μm,进一步优选5-100μm,特别优选10-75μm。
<聚酯膜的表面粗糙度>
本发明的阻燃性双轴取向聚酯膜的表面粗糙度Ra(中心线平均粗糙度)优选为0.1μm以上且低于2μm。表面粗糙度Ra的上限更优选低于1.5μm,进一步优选低于1.0μm,特别优选低于0.5μm。表面粗糙度Ra的下限可以是0.2μm以上,可进一步为0.3μm以上。更优选的表面粗糙度Ra的范围为0.1μm以上且低于1.5μm,进一步优选0.1μm以上且低于1.0μm,特别优选0.1μm以上且低于0.5μm。在本发明的阻燃成分的含量较多的区域可以是0.2μm以上且低于1.5μm、0.3μm以上且低于1.0μm、或0.3μm以上且低于0.5μm。
本发明的阻燃性双轴取向聚酯膜的Rmax(最大高度)优选为低于3μm,更优选为低于2.5μm,进一步优选为低于2.0μm。
所述表面粗糙度通过以特定量使用为上述的平均粒径、且除去了粗大颗粒的由次膦酸盐类形成的阻燃性颗粒来获得。
本发明的阻燃性双轴取向聚酯膜通过具有所述表面粗糙度Ra,经由热封层或粘合层等与其它层层合时的粘合性提高,例如可适宜地用于柔性电路基板、扁平电缆、太阳能电池背板等的用途。而如果粗大颗粒的存在导致Rmax超过上限,则制膜性和膜的机械强度欠缺。
并且,进而本发明的阻燃性双轴取向聚酯膜具有0.1μm以上且低于0.5μm的表面粗糙度Ra时,膜平坦性优异,因此在作为柔性电路基板使用时可以使金属层的电路图案高精细化。
<膜的机械强度>
本发明的阻燃性双轴取向聚酯膜的机械强度优选为150MPa以上,更优选160MPa以上,进一步优选170MPa以上,特别优选180MPa以上。所述膜机械强度通过使配合在聚酯膜中的阻燃剂颗粒的平均粒径在上述范围内、且将最大长度10μm以上的粗大颗粒降低为10个/m2以下来获得。
<耐水解性>
本发明的阻燃性双轴取向聚酯膜优选在121℃、2个气压的饱和水蒸气中处理10小时后的聚酯膜拉伸强度保持率为80%以上。所述膜拉伸强度保持率进一步优选为85%以上。所述拉伸强度保持率是指聚酯膜的膜连续制膜方向(以下可称为长度方向、纵向、MD方向)或与其垂直相交的方向(以下可称为宽度方向、横向、TD方向)中的至少一个方向的拉伸强度保持率,进一步优选两个方向均满足。
本发明的阻燃性双轴取向聚酯膜通过使用本发明的次膦酸盐类作为阻燃成分,并控制其平均粒径和膜中所含的粗大颗粒的数目,在阻燃性优异的同时也具有优异的耐水解性,湿热处理后仍可保持高的膜拉伸强度保持率。
<膜制造方法>
本发明的阻燃性双轴取向聚酯膜的制造可采用公知的制膜方法制造,例如可按照以下方法制造:将含有次膦酸盐的聚酯充分干燥,然后以熔点至(熔点+70)℃的温度在挤出机内熔融,通过T模头熔融挤出,将膜状熔融物在冷却辊(流延转鼓)上骤冷,制成未拉伸膜,接着将该未拉伸膜依次或同时双轴拉伸,热定型。通过依次双轴拉伸制膜时,将未拉伸膜沿纵向在60-170℃下、以2.3-5.5倍、更优选2.5-5.0倍的范围拉伸,接着用拉幅机(ステンター)沿横向在80-170℃下、以2.3-5.0倍、更优选2.5-4.8倍的范围拉伸。
热定型处理优选在180-260℃、更优选190-240℃的温度下、在拉紧下或限制收缩下进行热定型,热定型时间优选1-1000秒。同时双轴拉伸时,可采用上述的拉伸温度、拉伸倍率、热定型温度等。热定型后也可进行松弛处理。
<阻燃性聚酯膜层合体>
本发明的阻燃性双轴取向聚酯膜可以以与金属层层合的阻燃性聚酯膜层合体的形式使用。这里,金属层包含在膜上形成为层状的形状、导线等的形状、电路等一定的图案形状等。
所述阻燃性聚酯膜层合体可以适宜地用于要求阻燃性或耐水解性的用途,例如可例举扁平电缆或柔性印刷电路基板等的用途。也可用于与金属层贴合的其它用途。
<柔性印刷电路基板>
本发明的阻燃性双轴取向聚酯膜及其层合体可用于柔性印刷电路基板。
用于所述用途时,优选在阻燃性双轴取向聚酯膜的一个面上层合金属层,作为柔性印刷电路基板使用。在本用途中使用的金属层可例举铜箔。金属层的接合方式、形状的具体方式没有特别限定,例如可以利用:将金属层在阻燃性双轴取向聚酯膜上层合,然后将金属层进行图案蚀刻的所谓的减成法(subtractivemethod);将金属在阻燃性双轴取向聚酯膜上镀成图案状的加成法(additivemethod);将冲压成图案状的金属层贴合在阻燃性双轴取向聚酯膜上的烫印箔(stampingfoil)等。
使用本发明的阻燃性聚酯膜层合体得到的柔性印刷电路基板中,聚酯膜本身的阻燃性非常高,在加工为与金属层层合使用的柔性印刷电路基板用途时,表现与阻燃性双轴取向聚酯膜本身同样高的阻燃性,并且具备充分的机械强度和耐水解性,因此作为柔性印刷电路基板的长期耐久性也优异。另外本发明的阻燃性双轴取向聚酯膜的弯折性也优异,因此加工为柔性印刷电路基板时的冲压性优异,且可同时实现阻燃性和弯折性,因此可获得柔性高的柔性印刷电路基板。
本发明的聚酯膜具有0.1μm以上且低于0.5μm的表面粗糙度Ra时,膜平坦性优异,因此作为柔性印刷电路基板使用时可以使金属层的电路图案高精细化。
本发明的阻燃性双轴取向聚酯膜及其层合体的反射率特性也优异,因此可用作LED的柔性印刷电路基板。
[实施例]
以下通过实施例详述本发明,但本发明并不只限定于这些实施例。各特性值按以下方法测定。如无特别限定,实施例中的份和%分别表示重量份和重量%。
(1)聚酯成分的种类和含量
通过1H-NMR测定,13C-NMR测定,确定了聚酯的成分以及共聚成分和各成分量。
(2)磷成分的种类
使用NMR和EPMA确定了磷成分的种类。
(3)磷原子浓度
对于聚酯膜,通过荧光X射线的发光强度计算磷原子浓度。
(4)阻燃剂颗粒的平均粒径
对于聚酯膜的截面,使用HIROXCo.,Ltd.(株式会社ハイロックス)数字显微镜KH-3000,以3500倍的倍率取样20个颗粒,测定各粒径中的最大长度,从20点中除去最小值和最大值,由18点的平均值求出平均粒径。
(5)粗大颗粒的大小、个数
使用万能投影仪,以透射照明放大至20倍,计数具有10μm以上的最大长度的颗粒数,按以下基准评价。测定面积设为1m2
○:具有10μm以上的最大长度的颗粒数为10个/m2以下
×:具有10μm以上的最大长度的颗粒数超过10个/m2。
(6)制膜性
通过膜制造工序中的过滤器压力的变化量(ΔP)进行评价
○:ΔP=低于0.5MPa/h
Δ:ΔP=0.5MPa/h以上且低于1.0MPa/h
×:ΔP=1.0MPa/h以上。
(7)机械特性
将样品膜切成宽10mm、长150mm,将样品安装于100mm夹具之间,按照JIS-C2151、以拉伸速度100mm/分钟的条件进行拉伸试验,读取断裂时的载荷伸长曲线的载荷、伸长率。测定进行5次,以平均值作为结果。断裂强度是将载荷除以拉伸前的样品截面积进行计算(MPa),断裂伸长率是以拉伸前的样品长度为100时的百分比(%)计算。测定在调节为温度23±2℃、湿度50±5%的室内进行。测定装置使用orientec公司(オリエンテック)制造的TENSILON(テンシロン)UCT-100型
○:断裂强度为150MPa以上
×:断裂强度低于150MPa。
(8)耐水解性
将膜切成150mm长×10mm宽,将切取的短条状的试样片在设定为121℃·2atm·湿润饱和模式·100%RH的环境试验机内用不锈钢制的夹子垂挂。然后,经过10小时后从环境试验机上取下试验片,测定拉伸强度。将膜长度方向作为测定方向,测定进行5次,求其平均值,按以下基准评价耐水解性。测定装置使用orientec公司(オリエンテック)制造的TENSILON(テンシロン)UCT-100型。
拉伸强度保持率(%)=(处理后的拉伸强度X/初期的拉伸强度X0)×100
(式中,拉伸强度X表示在121℃、2atm、100%RH条件下处理规定时间后的拉伸强度,拉伸强度X0表示处理前的初期拉伸强度)
○:10小时后的拉伸强度保持率为80%以上
Δ:10小时后的拉伸强度保持率为50%以上且低于80%
×:10小时后的拉伸强度保持率低于50%。
(9)燃烧性
按照UL-94VTM法评价膜样品。将样品切成20cm×5cm,在23±2℃、50±5%RH中放置48小时,然后将试样下端距离喷灯上方10mm垂直地保持。以内径9.5mm、火焰长19mm的本生灯作为加热源,将该试样的下端与火焰接触3秒,按照VTM-0、VTM-1、VTM-2的评价基准评价阻燃性,在n=5的测定次数中,取相同等级的数目最多的等级。
(10)表面粗糙度Ra、Rmax
使用株式会社小坂研究所制造的触针式表面粗糙度计(SURFCORDERSE-30C),按照以下条件对聚酯膜表面进行测定,测定所计算出的中心线平均粗糙度Ra、最大高度Rmax,使用测定4次的平均值,按下述评价基准进行评价。在中心线平均粗糙度Ra(A评价)中评价为○时,也一并记录进一步细分的基准(B评价:○++、○+)。
<测定条件>
测定长度:2.5mm
截止值:0.25mm
测定环境:室温、大气中
<Ra(A评价)>
○:0.1μm以上且低于2μm
×:低于0.1μm或2μm以上
<Ra(B评价)>
○++:0.1μm以上且低于0.5μm
○+:0.5μm以上且低于2μm
<评价基准:Rmax>
○:低于3μm
×:3μm以上。
[实施例1]
使用特性粘度0.60dl/g、末端羧基浓度25当量/吨的聚对苯二甲酸乙二醇酯(酯交换催化剂:乙酸锰四水盐,聚合催化剂:三氧化锑)作为聚酯,将以聚酯膜的重量为基准、含有5重量%二甲基次膦酸铝(表1中记载为磷化合物A,平均粒径2μm,将粗大颗粒(最大长度10μm以上)通过粉碎、分级加工除去)的组合物在170℃干燥机中干燥3小时,然后加入到挤出机中,在熔融温度280℃下熔融混炼,由280℃的模头狭缝挤出,然后在表面温度设定为25℃的流延转鼓上冷却固化,制作未拉伸膜。
将该未拉伸膜导至加热为100℃的辊组中,沿长度方向(纵向)以3.5倍拉伸,在25℃的辊组中冷却。接着将纵向拉伸的膜的两端用夹具夹持,同时导入拉幅机,在加热为120℃的气氛中沿与长度方向垂直的方向(横向)以3.8倍拉伸。然后在拉幅机内进行230℃的热定型,在180℃下沿宽度方向松弛2%,然后均匀缓慢地冷却,冷却至室温,得到50μm厚的双轴拉伸膜。所得膜的特性示于表1中。本实施例的膜的阻燃性、机械特性、耐水解性优异。表面粗糙度的指标之一的Ra为0.10μm,Rmax为1.8μm,制膜性和机械特性优异。
[实施例2]
将阻燃剂变更为二乙基次膦酸铝(表1中记载为磷化合物B,平均粒径2μm,将粗大颗粒(最大长度10μm以上)通过粉碎、分级加工除去),除此之外进行与实施例1同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例3]
将阻燃剂的含量变更为3重量%,除此之外进行与实施例2同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例4]
将阻燃剂的含量变更为10重量%,除此之外进行与实施例2同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例5]
将阻燃剂的含量变更为15重量%,除此之外进行与实施例2同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例6]
将阻燃剂的含量变更为30重量%,除此之外进行与实施例2同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例7]
使用特性粘度0.57dl/g、末端羧基浓度25当量/吨的聚2,6-萘二甲酸乙二醇酯(酯交换催化剂:乙酸锰四水盐,聚合催化剂:三氧化锑)作为聚酯,将以聚酯膜的重量为基准含有5重量%二乙基次膦酸铝(磷化合物B,平均粒径2μm,将粗大颗粒(最大长度10μm以上)通过粉碎、分级加工除去)的组合物在180℃的干燥机中干燥5小时,然后加入到挤出机中,在熔融温度300℃下熔融混炼,由300℃的模头狭缝挤出,然后在表面温度设定为60℃的流延转鼓上冷却固化,制作未拉伸膜。
将该未拉伸膜导入加热为140℃的辊组中,沿长度方向(纵向)以3.5倍拉伸,在60℃的辊组中冷却。接着将纵向拉伸的膜的两端用夹具夹持,同时导入拉幅机,在加热为150℃的气氛中沿与长度方向垂直的方向(横向)以3.5倍拉伸。然后在拉幅机内进行230℃的热定型,在180℃下沿宽度方向松弛2%,然后均匀缓慢地冷却,冷却至室温,得到50μm厚的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例8]
将阻燃剂的含量变更为15重量%,除此之外进行与实施例7同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[实施例9]
将阻燃剂的平均粒径由2μm变更为3μm,除此之外进行与实施例2同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本实施例的膜的制膜性、阻燃性、机械特性和耐水解性均优异。
[比较例1]
不添加阻燃剂,除此之外进行与实施例1同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本比较例的膜的制膜性、机械特性、耐水解性、外观性优异,但阻燃性不充分。
[比较例2]
将阻燃剂的含量变更为45重量%,除此之外进行与实施例1同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本比较例中,制膜性不足,无法获得双轴拉伸膜。
[比较例3]
作为阻燃剂,变更为未除去粗大颗粒的二乙基次膦酸铝(表1中记载为磷化合物B’,平均粒径2μm),除此之外进行与实施例4同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本比较例中,制膜性不足,所得双轴拉伸膜表面粗糙,机械特性、耐水解性也低。
[比较例4]
作为阻燃剂,变更为未除去粗大颗粒的二乙基次膦酸铝(表1中记载为磷化合物B’,平均粒径30μm),除此之外进行与实施例4同样的操作,得到厚度50μm的双轴拉伸膜。所得膜的特性示于表1。本比较例中,制膜性不足,所得双轴拉伸膜表面粗糙,机械特性、耐水解性也低。
[表1]
表1中,PET表示聚对苯二甲酸乙二醇酯,PEN表示聚2,6-萘二甲酸乙二醇酯。
产业实用性
本发明的阻燃性双轴取向聚酯膜的制膜性优异,不会使聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯这样的聚酯所具有的机械特性或耐水解性降低,具备高阻燃性,因此可适宜地用于例如柔性印刷电路基板、扁平电缆、太阳能电池用背板等。
Claims (7)
1.阻燃性双轴取向聚酯膜,其特征在于:以聚酯膜重量为基准,含有70重量%以上99.5重量%以下的聚对苯二甲酸乙二醇酯或聚萘二甲酸乙二醇酯、以及0.5重量%以上30重量%以下的下式(1)或下式(2)所示的平均粒径0.5-3.0μm的阻燃剂颗粒,且该聚酯膜中所含的最大长度10μm以上的粗大颗粒的个数为10个/m2以下,
[化1]
式中,R1、R2为氢、碳原子数1-6的烷基和/或芳基,M表示金属,m表示M的价数;
[化2]
式中,R3、R4为氢、碳原子数1-6的烷基和/或芳基,R5为碳原子数1-6的亚烷基或碳原子数6-10的亚芳基、烷基亚芳基或芳基亚烷基,M表示金属,n表示M的价数。
2.权利要求1所述的阻燃性双轴取向聚酯膜,其中,所述聚酯膜的机械强度为150MPa以上。
3.权利要求1所述的阻燃性双轴取向聚酯膜,其中,在121℃、2个气压的饱和水蒸汽中处理10小时后,所述聚酯膜的拉伸强度保持率为80%以上。
4.权利要求1所述的阻燃性双轴取向聚酯膜,其中,所述聚酯膜的表面粗糙度Ra为0.1μm以上且低于0.5μm。
5.阻燃性聚酯膜层合体,该层合体是权利要求1-4中任一项所述的阻燃性双轴取向聚酯膜与金属层层合而成。
6.权利要求5所述的阻燃性聚酯膜层合体,该层合体用于柔性印刷电路基板用。
7.柔性电路基板,该柔性电路基板使用权利要求5所述的阻燃性聚酯膜层合体。
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