CN107275511A - 可固化封装剂及其用途 - Google Patents
可固化封装剂及其用途 Download PDFInfo
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- CN107275511A CN107275511A CN201710356983.6A CN201710356983A CN107275511A CN 107275511 A CN107275511 A CN 107275511A CN 201710356983 A CN201710356983 A CN 201710356983A CN 107275511 A CN107275511 A CN 107275511A
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- curable encapsulant
- encapsulant
- weight
- curable
- acrylate
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Classifications
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/80—Constructional details
- H10K30/88—Passivation; Containers; Encapsulations
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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- C—CHEMISTRY; METALLURGY
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Abstract
本发明涉及可固化封装剂及其用途,特别地涉及用于电子器件的具有压敏粘合性的可固化阻隔性封装剂或密封剂。所述封装剂特别适合于要求较低层压温度分布的有机电子器件。所述封装剂保护有机电子器件内的活性有机/聚合物组分免受环境因素如湿气和氧气的影响。
Description
本申请是2013年4月2日递交的国际申请号为PCT/US2013/034893、中国国家申请号为201380028831.3的申请的分案申请。
发明领域
本发明涉及用于电子器件且具有压敏粘合性的可固化的阻隔性封装剂或密封剂。其特别适合于有机电子器件封装。所述封装剂保护有机电子器件内的活性有机或聚合的(在下文中可交换使用)组分免受环境因素如湿气和氧气的影响。
发明背景
有机电子器件和电路如有机光伏电池(OPV)、有机发光二极管(OLED)、有机电泳显示器、有机电致变色显示器等在社会和商业用途中正变得越来越流行。例如,OLED在虚拟视图和直接视图显示器如笔记本电脑、电视、数字式电子表、电话、传呼机、蜂窝式电话、计算器/大面积装置中具有实用性。
已知各种各样的封装几何形状用于有机电子器件和电路,并且一般说来,这些几何形状由设置在基板/背板(在下文中可交换使用)和盖板/前板(在下文中可交换使用)之间的活性有机组分组成,所述基板与盖板用封闭所述活性有机组分的层压粘合剂或封装剂粘合到一起。基板和盖板之一或两者由透明材料例如透明玻璃和柔软的薄塑料膜制成。所述活性有机组分被粘附至所述基板,并且在一些实施方式中,其被在周边密封所述组分与基板之间接触区域的无机阻隔性涂层、缓冲膜或由无机和/或有机层组成的涂层覆盖。在活性有机组分上和在阻隔性涂层(存在时)上施加封装剂。该封装剂填充所述基板与盖板之间的空间,封闭所述活性有机组分并将所述基板粘附至盖板。在一些实施方式中,小袋或薄膜或厚膜形式的干燥剂包装被粘附至所述盖板,通常在盖板的缺口或空腔中,或者所述干燥剂设置在盖板内的凹槽中。
有机电子器件内的多数活性有机组分对由湿气和氧气引起的降解敏感。例如,简单来说,OLED由阳极、发光层和阴极组成。低功函数金属层通常用作阴极,以确保高效的电子注入和低操作电压。低功函数金属对氧气和湿气具有化学反应性,并且此类反应将限制装置的使用期限。氧气和湿气还将与发光有机材料反应,并抑制发光。因此,设计包围所述活性有机组分的封装,以限制氧气和水蒸气从环境向所述活性有机组分传输。
具有压敏粘合性的封装剂可用于限制氧气和水蒸气的传输,并且所述压敏粘合剂通常以薄膜提供在两个硅酮离型载体膜(衬垫)之间作为封装剂膜。在除去衬垫之一时,暴露的封装剂膜粘附至装置的盖板或基板。随后,除去第二衬垫,以使所述盖板和基板相互层压(或连接)。所述封装剂膜在长期暴露于应力时必须保持粘合性和柔软性。
具有压敏粘合性的封装剂膜或封装剂(在下文中可交换使用)可促进装置的生产量。虽然改进具有压敏粘合性的封装剂的制造速度和毒性,但是由于膜在装配温度下通常具有高于其液体封装剂对应物的粘度,因而缺点包括在装配期间的差的润湿性和空隙形成。对于含有组件如电极、母线、油墨行程(ink steps)、集成电路、电线等的基板,该问题由于其不规则表面而加重。为了获得更好的润湿性和使空隙形成减到最少,通常向未固化的封装剂膜施加热层压。然而,有机组分对热敏感,长时间暴露于热对所述组分有害。此外,由于所述封装剂是压敏粘合剂膜,因而所述膜在长期储存期间必须在室温下保持最小的冷流。
WO 2009/148722和WO 2011/062932公开了使用高重均分子量(Mw)(通常大于300,000道尔顿(Da))的聚异丁烯系封装剂。这种封装剂产生具有高粘度的压敏粘合剂膜,因而对有机电子器件中的空隙或气泡敏感。虽然可升高施加温度以使该问题最小化,但是活性有机组分在约120℃下开始分解。此外,由如此高Mw制成的封装剂通过溶液流延形成,并且除非利用极端温度和压力,否则不以热熔体形式挤出。
JP2012057065公开了具有压敏粘合性的不可固化的封装剂。为了适当地湿润具有组分的基板和使空隙形成减到最少,所述封装剂膜的粘度必须保持在120℃下低于1,000,000cps或低于200,000Da粘均分子量(Mv)。此外,所述热塑性封装剂在装置使用期限期间在应力下显示出冷流。
因此,现有技术中需要可在低于120℃的温度下层压、保持良好的粘合性、在具有不规则表面的基板上润湿、使冷流减到最少和形成无空隙的封装,同时允许基板在长期暴露于应力下具有柔软性的可固化封装剂膜。本发明满足该需要。
发明内容
本发明提供可辐射或热固化的封装剂,其适合于密封和粘合有机电子器件的基板和盖板以保护所述装置的活性有机组分免受湿气和氧气的影响。所述可辐射或热固化的封装剂具有允许所述装置在长期暴露于应力时保持柔软性和抗蠕变性的压敏特性。所述封装剂包含阻隔性橡胶、辐射或热反应性的阻隔性树脂和自由基引发剂。所述封装剂可进一步包含稀释剂、蜡、抗氧剂和/或干燥剂填料。
在一个实施方式中,所述可固化封装剂包含:
(a)Mw为约1,000至约95,000Da的聚异丁烯(PIB);
(b)官能化聚异丁烯,其具有(i)约1,000至约95,000Da的Mw(重均分子量)和(ii)多于一个的自由基反应性官能团,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯组成的组;和
(c)自由基引发剂。
所述封装剂基本上不含Mw小于约1,000Da的任何丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物,并且所述封装剂基本上不含增粘剂。在这里,术语"基本上不含"是指,基于整个封装剂组合物,所述封装剂含有小于5,000ppm(百万份之一)。所述可固化封装剂可进一步包含官能化聚烯烃,所述官能化聚烯烃具有(i)约1,000至约95,000Da的Mw和(ii)含有多于一个自由基反应性官能团的官能化聚异丁烯,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯组成的组。
在另一个实施方式中,所述可固化封装剂包含:
(a)Mw为约1,000至约95,000Da的聚异丁烯;
(b)官能化聚烯烃,其具有(i)约1,000至约95,000Da的Mw和(ii)多于一个的自由基反应性官能团,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯组成的组;和
(c)自由基引发剂。
所述封装剂基本上不含Mw小于约1,000Da的任何丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物,并且所述封装剂基本上不含增粘剂。
在另一个实施方式中,所述可固化封装剂包含:
(a)190℃下的布氏粘度小于8,000cps的非结晶性聚α烯烃;
(b)官能化聚烯烃,其具有(i)约1,000至约95,000Da的Mw和(ii)含有多于一个自由基反应性官能团的官能化聚异丁烯,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯组成的组;和
(c)自由基引发剂;和
(d)增粘剂。
所述封装剂基本上不含Mw小于约1,000Da的丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物。
对于上述可固化封装剂,所述自由基引发剂选自由光引发剂和热引发剂的组成的组。具有光引发剂的可固化封装剂通常以热熔体形成,所述封装剂130℃下的布氏粘度在约10,000至约900,000cps范围内。具有热引发剂的可固化封装剂通常是溶液流延,所述封装剂在80℃下的布氏粘度在约10,000至约900,000cps的范围内。
在另一个实施方式中,所述可固化封装剂是通过在80℃至约150℃下混合所述封装剂的上述组分直到形成均匀的熔体,挤出或流延所述熔体至厚度为约0.01mm至约10mm的膜并冷却所述膜而形成的。
在另一个实施方式中,所述可固化封装剂是通过在室温下将所述封装剂的上述组分与溶剂混合直到形成均匀混合物,流延所述混合物至厚度为约0.01mm至约10mm的膜,并蒸发或馏出所述溶剂而形成的。
另一个实施方式涉及一种形成固化的封装剂器件的方法,其包含下述步骤:
(1)在约50至约120℃的温度下,将上述可固化封装剂施加到基板的至少一部分上;
(2)将盖板施加到所述可固化封装剂上;和
(3)使所述可固化封装剂固化
由此所述封装剂固化并将所述基板粘合至所述盖板。通过UV照射和/或热辐射进行所述可固化封装剂的固化。在另一个实施方式中,首先在步骤(1)中将所述可固化封装剂施加到所述盖板上,和在步骤(3)中,将所述基板施加到所述可固化封装剂上。
另一实施方式涉及包含上述固化的封装剂的器件。器件包括电子、光电子、OLED、光伏电池、有机光伏电池、柔软性薄膜有机光伏电池、CIGS光伏电池等。
附图说明
图1为布氏粘度曲线。
详细说明
在此引用的所有参考文献以其整体方式通过引用并入。
在此的术语辐射固化是指所述封装剂的可固化部分通过光化辐射暴露而韧化、硬化或硫化。光化辐射是诱导材料中化学变化的电磁辐射,为了本说明书和权利要求范围内的目的,将包括电子束固化。在大多数情况下,此类辐射为紫外线(UV)或可见光。通过添加合适的光引发剂实现该固化的引发。所述封装剂的固化是通过直接暴露于紫外线(UV)或可见光或者通过由聚酯、聚碳酸酯、玻璃等制成的透明罩或盖板间接暴露来实现。
术语热固化是指所述封装剂的可固化部分通过暴露至烘箱、红外线(IR)、近IR或微波的加热而韧化、硬化或硫化。热固化温度在50-200℃、优选100-170℃之间。
聚异丁烯(PIB)和PIB稀释剂实质上是异丁烯的均聚物。它们也可称为聚丁烯和丁基橡胶。它们通常每个聚合物链含有小于75%的末端α-烯烃。所述PIB和PIB稀释剂不含任何其它自由基反应性官能团,该官能团包括但不限于丙烯酸酯、(甲基)丙烯酸酯、苯乙烯C=C键、二烯丙基、马来酸酐等。可商购获得的PIB和PIB稀释剂包括,但不限于Oppanol、Glissopal和Indopol。虽然许多这些PIB可含有甚至高达75%末端αC=C键,但这些PIB对自由基反应的反应性较低且不完全,因此认为是非反应性或非可固化的PIB。此外,PIB和PIB稀释剂的重均分子量(Mw)在约1,000至约95,000Da的范围内。PIB稀释剂的Mw通常在约1,000至约10,000Da的范围内。在所述封装剂中优选这些低Mw和低粘度PIB聚合物,以实现100%润湿和可涂布热熔体。
基于所述可固化封装剂的总重量而不考虑任何溶剂,所述可固化封装剂中的PIB的量为约10至约90重量%,更优选约70-90重量%。
示例性的非结晶性聚α烯烃(APAO)包括乙烯、丙烯和丁烯的无规共聚物或三元共聚物的聚合物和其它基本上非结晶性或半结晶性聚合物。适合地,所述APAO包括约20%至约80%的共聚物或三元共聚物和约20%至约80%的其它基本上非结晶性或半结晶性丙烯-乙烯聚合物。或者,所述APAO包括约40%至约60%的共聚物或三元共聚物和约40%至约60%的其它基本上非结晶性或半结晶性丙烯-乙烯聚合物。APAO可以是190℃下的布氏粘度小于8,000cps的1-丁烯与乙烯或丙烯的共聚物或1-丁烯与乙烯和丙烯的三元共聚物。所述1-丁烯共聚物应包括约20重量%至约65重量%的1-丁烯或约30重量%至约55重量%的1-丁烯。或者,所述APAO可包括具有最多80%乙烯的乙烯-丙烯共聚物。商购适合的APAO包括Rextac(Rexene LLC)、Eastoflex(Eastman Corporation)、Vestoplast(EvonikCorporation)。适合的APAO在190℃的粘度小于8,000cps。熔点低于约100℃的茂金属催化的半结晶性聚烯烃也可适合于所述可固化封装剂和代替使用齐格勒纳塔催化剂的APAO。示例性的低熔点半结晶性聚烯烃包括重均分子量小于约100,000Da且多分散指数小于约3的C2-C6聚烯烃。这些低熔点半结晶性聚烯烃可以Linxar系列从Exxon Mobil商购获得。
基于所述可固化封装剂的总重量而不考虑任何溶剂,所述可固化封装剂中的APAO的量为约10重量%至约90重量%,更优选约70-90重量%。
示例性的官能化PIB包括,但不限于,二烯丙基聚异丁烯、二(甲基)丙烯酸酯聚异丁烯和乙烯基封端的聚异丁烯。代表性的聚异丁烯(甲基)丙烯酸酯描述在授予EdisonPolymer Innovation Corp.的美国专利5,171,760、授予Dow Corning Corp.的美国专利5,665,823以及T.P.Liao和J.P.Kennedy的Polymer Bulletin,Vol.6,pp.135-141(1981)中。代表性的聚异丁烯乙烯基醚描述在Polymer Bulletin,Vol.25,pp.633(1991),J.P.Kennedy和授予Dow Corning Corp的美国专利6,054,549、6,706,779B2中。优选的官能化PIB为自由基反应性的聚异丁烯、丁基橡胶衍生物等,其用(甲基)丙烯酸类或75%的α-烯烃官能团封端或接枝。特别是,所述官能化聚异丁烯具有(i)约1,000至约95,000Da的Mw和(ii)每个聚合物链含有多于一个的自由基反应性官能团。所述官能化PIB是用选自末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯的自由基官能团形成的。
本发明中的官能化聚烯烃包括自由基反应性的(甲基)丙烯酸类封端和侧链接枝的、丁二烯、异戌二烯、乙烯、丙烯、丁烯和衍生物的官能化低聚物、聚合物或无规共聚物。所述官能化聚烯烃具有约1,000至约95,000Da的Mw,并在聚合物链中含有多于一个的自由基反应性官能团。所述官能化聚烯烃是用选自末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯的自由基官能团形成的。所述官能化烯烃是用选自末端(甲基)丙烯酸酯、侧链(甲基)丙烯酸酯、末端丙烯酸酯和/或侧链丙烯酸酯的自由基官能团形成的。示例性的官能化低聚物、聚合物或共聚物包括,但不限于,二(甲基)丙烯酸酯化-聚丁二烯、二(甲基)丙烯酸酯化-聚异戊二烯、氢化二(甲基)丙烯酸酯化-聚丁二烯、氢化二(甲基)丙烯酸酯化-聚异戊二烯,其中许多可从Sartomer和Kuraray获得。"(甲基)丙烯酸酯化"在此定义为用丙烯酸酯或甲基丙烯酸酯官能化。在其它实施方式中,其它反应性液体低聚物和/或聚合物被(甲基)丙烯酸酯化并可部分用于代替可固化的官能化聚烯烃,它们包括,但不限于,(甲基)丙烯酸酯化-聚氨酯、(甲基)丙烯酸酯化聚氨酯低聚物、和(甲基)丙烯酸酯化-聚酯、(甲基)丙烯酸酯化苯乙烯-丁二烯共聚物、(甲基)丙烯酸酯化丙烯腈-丁二烯共聚物、(甲基)丙烯酸酯化聚硅氧烷、(甲基)丙烯酸酯化EPDM橡胶(乙烯丙烯二烯共聚物)、(甲基)丙烯酸酯化丁基橡胶、(甲基)丙烯酸酯化溴化丁基橡胶(溴化异丁烯-异戌二烯共聚物)、(甲基)丙烯酸酯化氯化丁基橡胶(氯化异丁烯-异戌二烯共聚物)。这些树脂可以没有(甲基)丙烯酸酯官能团商购获得并可由本领域技术人员不经过度实验进行官能化。
基于所述可固化封装剂的总重量而不考虑任何溶剂,所述可固化封装剂中的官能化PIB的量为约5重量%至约90重量%,更优选约10-50重量%。
反应性PIB或反应性聚烯烃中具有反应性且可通过辐射或加热固化的末端和/或接枝侧链官能团的实例包括但不限于选自由丙烯酸酯基、甲基丙烯酸酯基、乙烯基、乙烯基醚基、丙烯基、巴豆基、烯丙基、硅氢化物基、乙烯基甲硅烷基、炔丙基、环烯基、巯基、缩水甘油基、脂族环氧基、环脂族环氧基、氧杂环丁烷基、衣康酸酯基、马来酰亚胺基、马来酸酯基、富马酸酯基、肉桂酸酯基、苯乙烯基、丙烯酰胺基、甲基丙烯酰胺基和查耳酮基组成的组的那些。
自由基固化引发剂包括通过电磁能射线如UV射线分解产生自由基的自由基聚合引发剂、或通过热分解产生自由基的可热分解的自由基引发剂。包含一种或多种光引发剂的自由基光聚合引发体系可在Fouassier,J-P.,Photoinitiation,Photopolymerizationand Photocuring Fundamentals and Applications 1995,Hanser/GardnerPublications,Inc.,New York,NY中找到。
所述自由基光聚合引发剂包括I型α裂解引发剂如苯乙酮衍生物如2-羟基-2-甲基苯丙酮和1-羟基环己基苯基酮;酰基膦氧化物衍生物如双(2,4,6-三甲基苯甲酰基)苯膦氧化物;和苯偶姻醚衍生物如苯偶姻甲醚和苯偶姻乙醚。可商购获得的自由基光引发剂包括来自Ciba Speciality Chemical的Irgacure 651、Irgacure 184、Irgacure 907、Darocur1173和Irgacure 819。II型光引发剂也适合于所述可固化封装剂,它们包括二苯甲酮、异丙基噻吨酮和蒽醌。也可使用上述化合物的许多取代衍生物。用于辐射可固化封装剂的光引发剂的选择是辐射固化领域的技术人员熟知的。所述光引发剂体系将包含一种或多种光引发剂和任选存在的一种或多种光敏剂。合适的光引发剂的选择高度取决于将使用所述封装剂的具体应用。适合的光引发剂是显示出与封装剂中树脂和其它添加剂的光吸收谱不同的光吸收谱的光引发剂。基于所述封装剂的总重量而不考虑溶剂,所述光引发剂的量通常在约0.01重量%至约10重量%的范围内,优选约0.01重量%至约5重量%。
在一个实施方式中,所述封装剂通过光学透明盖板或前板固化,所述光引发剂必须能够吸收可穿过所述盖板或基板的波长下的辐射。例如,如果封装剂通过钠钙玻璃盖板固化,则所述光引发剂必须具有高于320nm的显著的UV吸光率。低于320nm的UV辐射将被钠钙玻璃盖板吸收并不会到达所述光引发剂。在该实例中,有益的是在光引发体系中包括红移光引发剂或与光引发剂一起的光敏剂,以增大转移至光引发剂的能量。如果封装剂通过具有低于400nm的截止吸光度(cut off absorbance)的阻隔性PET膜固化,则所述光引发剂必须具有高于400nm的UV吸光度。此类光引发剂的实例包括,但不限于,可从BASF商购获得的819、2022、Lucirin TPO或TPO-L。
可热固化的自由基聚合引发剂包括过氧化物,如过氧化-2-乙基-已酸1,1,3,3-甲基丁酯、1,1-双(叔丁基过氧基)环己烷、1,1-双(叔丁基过氧基)环十二烷、过氧化间苯二甲酸二叔丁基酯、过氧化苯甲酸叔丁基酯、二异丙苯基过氧化物、叔丁基异丙苯基过氧化物、2,5-二甲基-2,5-二(叔丁基过氧基)己烷、2,5-二甲基-2,5-二(叔丁基过氧基)-3-己炔和异丙苯氢过氧化物。基于所述封装剂的总重量而不考虑溶剂,所述自由基热引发剂的量通常在约0.01重量%至约10重量%的范围内。
在一个实施方式中,期望选择热固化引发剂以提供适当的引发温度,其足够高以防止过早交联,而且足够低以防止电子器件暴露于过高温度。这种过高温度可能使所述器件内的反应性有机组分分解。适合的可商购获得的自由基热引发剂的实例包括,但不限于,来自United Initiators的LUPEROX TBEC、来自Akzo Nobel Polymer Chemicals的TRIGONOX 101和TRIGONOX 201、来自Arkema的LUPEROX 101和LUPEROX 231、来自GEOSpecialty Chemicals的DICUP、2,5,-二甲基-2,5双(叔丁基过氧基)己炔-3如可根据商标名称LUPEROX 130从Arkema获得的那些、来自Akzo Nobel Polymer Chemicals的TRIGONOX145;二叔丁基过氧化物如可根据商标名称TRIGONOX B从Akzo Nobel Polymer Chemicals获得的那些。基于所述封装剂的总重量而不考虑溶剂,适合的热自由基引发剂的量在约0.01重量%至约10重量%的范围内。这些自由基引发剂的典型固化温度通常在约130℃至约200℃的范围内,但是可提高温度以更快地固化。
在一些实施方式中,无机填料可用于改进所述封装剂的湿气和氧气阻隔性能。代表性的填料包括,但不限于,石英粉、熔融二氧化硅、无定形二氧化硅、滑石、玻璃珠、石墨、炭黑、氧化铝、粘土、石墨烯、纳米粘土、云母、氮化铝和氮化硼。由银、铜、金、锡、锡/铅合金以及其它合金组成的金属粉末和薄片也是用于导电应用的适合填料。也可使用有机填料粉末如聚(四氯乙烯)、聚(三氟氯乙烯)、聚(偏二氯乙烯)。适合用于可自由基固化封装剂的此类填料的类型和量属于本领域技术人员的专业知识。然而,一般地,此类填料的含量将在整个封装剂的0.5重量%至50重量%的范围内,不考虑溶剂。
在另一个实施方式中,干燥剂可用于改进封装剂的湿气阻隔性。当添加时,干燥剂构成至多20重量%的不包括溶剂在内所述封装剂。适合使用的具有干燥剂性质的填料(称为干燥剂填料)可以是提供适合的湿气清除速率、容量和残留湿气水平(所述干燥剂可主动清除水的最低湿气水平)以符合特定电子器件允许的湿气含量的那些填料中的任一种。所述干燥剂填料将能够与水和/或水蒸气反应、吸收或吸附水和/或水蒸气。此类干燥剂的代表性清单可在Dean,J.Lange's Handbook of Chemistry,1999,McGraw Hill,Inc.,NewYork,NY,pp.11.5中找到。
一般说来,适合的干燥剂包括金属氧化物如CaO、BaO、MgO;其它氧化物如SiO2、P2O5、Al2O3;金属氢化物如CaH2、NaH、LiAlH4;金属盐如CaSO4、Na2SO4、MgSO4、CaCO3、K2CO3和CaCl2;粉末沸石如4A和3A分子筛;金属高氯酸盐如Ba(ClO4)2、Mg(ClO4)2;超吸收性聚合物如轻度交联的聚(丙烯酸);和与水反应的金属如钙。与任何填料一样,干燥剂填料粒径、粒径分布、形状和表面官能团将影响其可装载到树脂体系中的水平和可能导致的流变性。上述因素为本领域技术人员所理解,并不以别的方式与本发明的组合物相关。以上公开的更常规的非干燥剂填料和这些干燥剂填料的混合物涵盖和描述在实施例中。所述干燥剂填料的常规粒径范围为约0.001微米至约200微米。本领域技术人员将能够确定特定最终用途应用所需的适合的树脂粒径范围、流变性和清除速率。
所述封装剂可进一步包含增塑剂、增粘剂、蜡和矿物油以调节配制物的粘度。
增塑剂的非限制性实例包括极性增塑剂、固体增塑剂、液体增塑剂(天然的和合成的),和在性质上主要是脂肪族且与PIB和聚烯烃相容的增塑剂。固体增塑剂在环境温度下为固体,优选具有大于60℃的软化点。任何随后能在封装剂中再结晶的固体增塑剂是适合的。实例包括可从Genovique Specialties获得的1,4-环己烷二甲醇二苯甲酸酯Benzoflex352。天然液体增塑剂的非限制性实例为植物油。合成液体增塑剂包括液体聚烯烃、中等至高分子量的异链烷烃或石蜡。实例包括来自ExxonMobil Chemical的SpectraSyn Plus 6。示例性的液体增粘剂(环球法软化点低于约25℃)为液体增粘稀释剂,包括聚萜烯,如可从Sartomer获得的Wingtack 10和可从ExxonMobil Chemical获得的Escorez 2520。合成的液体低聚物为永久性呈流体形式的、聚丁烯、聚丙烯、聚萜烯等的高粘度低聚物。实例包括可作为LIR 50从Kuraray获得的聚异戊二烯、可根据名称Indopol获得的Amoco的聚丁烯、来自Sartomer的Wingtack 10和合成的液体低聚物聚丁烯如来自Amoco的Indopol 300。
适合的增粘剂包括,但不限于,与PIB或其聚烯烃相容的任何树脂或混合物,例如(1)天然或改性的松香,例如脂松香、木松香、妥尔油松香、蒸馏的松香、氢化松香、二聚松香和聚合松香;(2)天然或改性松香的甘油和季戊四醇酯,例如,浅色木松香的甘油酯、氢化松香的甘油酯、聚合松香的甘油酯、氢化松香的季戊四醇酯和松香的苯酚改性的季戊四醇酯;(3)天然萜烯的共聚物和三元共聚物,例如苯乙烯/萜烯和D-甲基苯乙烯/萜烯;(4)通过ASTM方法E28,58T测定的软化点为约80℃至约150℃的聚萜烯树脂;后者聚萜烯树脂通常由萜烃如被称为蒎烯的双环单萜在弗瑞德-克来福特催化剂存在下,在适当的低温下聚合得到;还包括氢化的聚萜烯树脂;(5)苯酚改性的萜烯树脂和其氢化衍生物,例如由双环萜烯和苯酚在酸性介质中缩合得到的树脂产物;(6)环球法软化点为约70℃至约135℃的脂族石油烃树脂;后者树脂由主要由烯烃和二烯烃组成的单体聚合得到;还包括所述氢化的脂族石油烃树脂;(7)脂环族石油烃树脂及其氢化的衍生物;和(8)脂族/芳香族或环脂族/芳香族共聚物及其氢化的衍生物。特定增粘剂的合意性和选择可取决于与阻隔膜配制物中其它组分的相容性。当存在时,基于所述封装剂的总重量而不考虑任何溶剂,本发明的封装剂组合物通常将包含小于约80重量%、通常约10重量%至约65重量%的量的增粘剂。
适合的与PIB或聚烯烃相容的蜡包括石油基常规蜡、天然型蜡、官能化的蜡和聚烯烃共聚物。术语石油衍生的蜡包括熔点在约130°F至约225°F范围内的石蜡和微晶蜡以及合成蜡如低分子量聚乙烯或费托蜡。最优选的是熔点为至少约175°F的聚乙烯蜡或费托蜡。基于所述封装剂的总重量而不考虑溶剂,获得期望性质所必需的蜡的量将通常在约0.5重量%至约10重量%的范围内。
油的非限制性实例包括石蜡族和环烷系石油,高度精制的工业级白凡士林矿物油如来自Crompton-Witco的Kaydol油和环烷系石油如来自Calumet Lubricants的Calsol5550。稀释剂也可以是液体增粘剂(环球法软化点低于约25℃)、合成的液体低聚物和它们的混合物。当存在时,基于所述封装剂的总重量而不考虑溶剂,本发明的配制物通常将包含小于约50重量%的量的油稀释剂。
所述可固化封装剂可任选包含添加剂,所述添加剂包括热稳定剂、抗氧剂、UV吸收剂和受阻胺光稳定剂。任何已知的热稳定剂可以是适合的,优选的常规种类热稳定剂包括,但不限于,酚类抗氧剂、烷基化单酚类、烷基硫代甲基酚类、氢醌类、烷基化氢醌类、生育酚类、羟基化硫代二苯基醚类、亚烷基双酚类、O-、N-和S-苄基化合物、羟基苯甲基化的丙二酸酯类、芳族羟基苄基化合物、三嗪化合物、胺类抗氧剂、芳基胺类、二芳基胺类、多芳基胺类、酰基氨基酚类、草酰胺类、金属钝化剂类、亚磷酸酯类、亚膦酸酯类、苯甲基膦酸酯、抗坏血酸(维生素C)、羟基胺类、硝酮类、硫代增效剂类、苯并呋喃酮类、吲哚满酮等,和它们的混合物。热稳定剂的使用是任选的,在一些情况下不是优选的,特别是如果其与电子器件内活性有机组分反应且使其分解。当使用热稳定剂时,基于所述封装剂的总重量而不考虑溶剂,它们可以以约0.00005重量%至至多约10重量%的水平存在。
任何已知的UV吸收剂可适用于所述封装剂组合物,优选的常规种类UV吸收剂包括,但不限于,苯并三唑衍生物类、羟基二苯甲酮类、羟苯基三嗪类、取代的和未被取代的苯甲酸酯等以及它们的混合物。可使用受阻胺光稳定剂(HALS),其也是本领域众所周知的。一般地,受阻胺光稳定剂是仲、叔、乙酰化、N-烃氧基取代的、羟基取代的N-烃氧基取代的或其它取代的环胺,其特征在于大量位阻,通常衍生自与胺官能团邻近的碳原子上的脂肪族取代。UV吸收剂的使用是任选的,在一些情况下不是优选的,特别是如果其与电子器件内活性有机组分反应且使其分解。当利用UV吸收剂时,基于所述可固化封装剂的总重量而不考虑溶剂,它们可以以约0.00005重量%至至多约10重量%的水平存在于所述配制物中。
可用于所述封装剂组合物的硅烷偶联剂的实例包括,但不限于,C3-C24烷基三烷氧基硅烷、(甲基)丙烯酰氧丙基三烷氧基硅烷、氯丙基甲氧基硅烷、乙烯基甲氧基硅烷、乙烯基乙氧基硅烷、乙烯基三甲氧基乙氧基硅烷、乙烯基苯甲基丙基甲氧基硅烷、氨基丙基三甲氧基硅烷、乙烯基乙酰氧基硅烷、缩水甘油醚氧基丙基三烷氧基硅烷、β-(3,4-环氧基环己基)乙基三甲氧基硅烷、巯基丙基甲氧基硅烷、氨基丙基三烷氧基硅烷和它们中的两种或更多种的混合物。硅烷偶联剂的使用是任选的,在一些情况下不是优选的,特别是如果其与电子器件内活性有机组分反应且使其分解。当使用硅烷偶联剂时,基于所述可固化封装剂的总重量而不考虑溶剂,它们可以以约0.01重量%至至多约10重量%的水平存在于所述配制物中。
通常用于压敏粘合剂以满足不同性质和符合特定应用要求的其它添加剂也可以添加到所述可固化封装剂中。此类添加剂包括,但不限于,颜料、流动改性剂、染料,取决于用途,其可以以较小或较大的量添加到所述封装剂组合物中。
所述可固化封装剂膜可以在基板(如PET、玻璃等)上或在载体膜(如硅酮PET或牛皮纸离型衬垫)之间的片或卷形式提供。包含封装剂膜的片或卷可通过任何适合的方法来制备。例如,所述片可通过溶液流延或浸涂来形成。使用本领域已知的技术准备溶液流延。封装剂组分通常全部溶于溶剂或溶剂的混合物以形成溶液,所述溶剂例如二甲苯、甲苯、庚烷、己烷、环己烷等。溶液以每平方米规定重量流延成膜,然后使溶剂蒸发,以形成固体封装剂膜。优选的方法是热熔体膜挤出、压塑、注塑、层压、吹膜法、串联挤出涂布、热熔体挤出流延、熔体共挤出流延或本领域技术人员已知的任何适合的熔融方法。使用本领域已知的技术制备热熔体。通常,通过在约50-190℃的温度下混合熔融的组分直到获得均匀的混合物来制备所述热熔体。混合温度应保持尽可能低以避免过早交联,其取决于特定的配制物和组分,特别是如果所述封装剂组合物是热固性的。各种混合方法是本领域已知的,任何制造均匀混合物的方法均是符合要求的。在热熔体膜涂布法中,所述热熔体的温度应保持低于150℃,以避免过早交联或分解。在一些膜挤出方法中,保持热熔体的温度等于或低于约120℃、110℃或甚至低于100℃。
所述可固化封装剂涂布在两个衬垫之间以形成具有压敏粘合性的无可固化封装剂的膜。所述可固化封装剂在涂布温度下,通常在约50℃至约200℃范围内,具有约10,000cps至约900,000cps的布氏粘度范围,优选在约100℃至约130℃下具有10,000cps至500,000cps的布氏粘度范围。这种粘度范围使得所述封装剂可热熔体涂布成膜。膜厚度在约0.01mm至约10mm、优选约0.03mm至约0.5mm的范围内。所述可固化封装剂膜在等于或低于35℃下仍然是压敏粘合剂膜,并且在储存时具有最小的冷流。
在移除第一衬垫时,用压力将暴露的可固化封装剂膜层压到前板或基板。随后,除去第二衬垫,并将所述封装剂膜层压到剩下的前板或基板。在一个实施方式中,将可固化封装剂膜同时层压到前板和基板。可施加加热(约50℃至约190℃,优选约80℃至约150℃)和/或真空以促进层压和除去任何夹带的空气并消除各层之间的任何空隙。在另一个实施方式中,由于基板上的有机活性组分在大于120℃的温度下开始分解,优选的层压温度范围低于约120℃,在一些应用中低于约110℃。然后,通过加热或UV照射固化所述可固化封装剂。可用约100℃至约190℃的温度完成热固化。用约280nm至约450nm的UV照射完成UV固化。
固化的封装剂膜在长期暴露于应力时保持柔软性和抗蠕变性。蠕变或冷流可表示在刚性显示器或光伏电池中在其长期弯曲或保持垂直时柔性显示器或薄膜光伏电池的剥离缺陷。
在一个实施方式中,所述封装剂膜在基板和盖板的两面上具有不规则表面以在层压过程中促进除气。可通过机械压印或在片挤出时熔体裂缝然后淬灭以在处理期间保留表面粗糙度来形成不规则表面。可通过众所周知的常规技术方法,将表面图案施加至片。例如,挤出片可在设置在紧靠着挤出机模头出口的模具辊的特别制备的表面上通过。这将期望的表面特征赋予离开模具的熔融聚合物的一侧。因此,当这种模具辊的表面具有微小的峰和谷时,这将粗糙表面赋予通过所述辊的聚合物片的一侧,所述粗糙表面通常将分别对应于所述辊表面的谷和峰。这种模具辊描述在例如美国专利第4,035,549号和美国专利公开号2003/0124296中。
在另一个实施方式中,所述封装剂膜可以是单层或多层形式。术语"单层"是指由本发明中描述的粘合剂制成或基本上由所述粘合剂构成的片。当呈多层形式时,所述片包含子层,至少一个所述子层由本发明的粘合剂制成或基本上由所述粘合剂构成,而其它子层可由任何其它适合的聚合物材料制成或包含任何其它适合的聚合物材料,例如α-烯烃与α,β-烯属不饱和羧酸的共聚物(即酸共聚物)、部分中和的离子酸共聚物(即离聚物)、乙烯/乙酸乙烯酯共聚物、聚乙烯醇缩醛(包括声学级聚乙烯醇缩醛)、聚氨酯、聚氯乙烯、聚乙烯(例如线性低密度聚乙烯)、聚烯烃嵌段共聚物弹性体、α-烯烃与α,β-烯属不饱和羧酸酯的共聚物(例如,乙烯丙烯酸甲酯共聚物和乙烯丙烯酸丁酯共聚物)、硅酮弹性体、环氧树脂和它们中两种或更多种的组合。
在另一个实施方式中,在此描述的可固化封装剂用作光伏电池模块用封装剂。在形成光伏电池时,将包含压敏粘合剂膜形式的可固化封装剂的封装剂片或卷层压到光伏电池模块组合件。所述光电池模块组合件包括可将光转化成电能的任何物品或材料。有用的光伏电池包括,但不限于,晶片型光伏电池(例如,c-Si或mc-Si型光伏电池)和薄膜光伏电池(例如,a-Si、c-Si、CdTe、硒化铜铟(CIS)、硒化铜铟镓(CIGS))、吸光染料或有机半导体型太阳能电池。在光伏电池模块组合件中,优选所述电池电学上互联或设置在平面中。另外,所述光伏电池模块组合件可进一步包含电线,如交叉带和母线。
所述光电池模块/电池(在此可互换使用)组合件可以是两面的。在这种实施方式中,位于光伏电池任一侧上的所有层压材料均应足够透明,以允许足够的阳光或反射的阳光到达所述光伏电池。或者,所述光伏电池可具有正面面向阳光侧(其也称为正面,在实际使用状态中,通常面向太阳)和背面非面向阳光侧(其也称为背面,在实际使用状态中,通常背向太阳)。所述光伏电池限定所述光伏电池组合件的前面和背面之间的边界。在这种组合件中,在位于太阳能电池组合件的正面面向阳光侧的层压层中存在的所有材料应具有足够的透明度,以允许足够的太阳光到达所述光伏电池。在位于所述光伏电池层的背面非面向阳光侧的层压层中存在的材料不必是透明的。所述光伏电池通常包含层压到太阳能电池组合件的至少一个包含所述封装剂的封装剂层。彼此"层压"的两种组分直接(即,在两层之间没有任何额外的材料)或间接(即,在两层之间具有额外的材料如中间层或粘合剂材料)结合。在某些层压体中,包含混合组合物的封装剂层直接结合至所述光伏电池层。
在一个实施方式中,所述光伏电池组合件具有含有峰和空隙的不规则表面。因此,在层压过程中,包含所述封装剂的封装剂片将熔融并溢出,以均匀的方式填充所述光伏电池组合件中的空隙。除非在有限的情况中另作说明,所述封装剂层的厚度为层压之前的封装剂层的厚度。然而,一般说来,最终光电池模块中的封装剂层保持约1密耳至约120密耳(约0.025mm至约3mm)、优选约2密耳至约40密耳(约0.05mm至约1mm)的平均总厚度。
所述光伏电池可进一步包含包埋在所述模块中的其它功能膜、片层、封装剂层(例如电介质层或阻隔层)。此类功能层可包含任何上述聚合物膜或涂有其它功能性涂层的那些。例如,涂有金属氧化物涂层的聚(对苯二甲酸乙二醇酯)(PET)膜,如美国专利第6,521,825和6,818,819号以及欧洲专利第1182710号中描述的那些,可用作层压体中的氧气和湿气阻隔层。其它封装剂层包含其它聚合物材料,如酸共聚物、离聚物、乙烯/乙酸乙烯酯共聚物、聚乙烯醇缩醛(包括声学级聚乙烯醇缩醛)、聚氨酯、聚氯乙烯、聚乙烯(例如线性低密度聚乙烯)、聚烯烃嵌段共聚物弹性体、α-烯烃与α,β-烯属不饱和羧酸酯的共聚物(例如,乙烯丙烯酸甲酯共聚物和乙烯丙烯酸丁酯共聚物)、硅酮弹性体、环氧树脂和它们中两种或更多种的组合。适合用于入射层或背衬层的膜包含聚合物,其包括但不限于,聚酯(例如,聚(对苯二甲酸乙二醇酯)和聚(萘二甲酸乙二醇酯))、聚碳酸酯、聚烯烃(例如,聚丙烯、聚乙烯和环状聚烯烃)、降冰片烯聚合物、聚苯乙烯(例如,间规聚苯乙烯)、苯乙烯-丙烯酸酯共聚物、丙烯腈-苯乙烯共聚物、聚砜(例如,聚醚砜、聚砜等)、尼龙、聚(氨基甲酸酯)、丙烯酸树酯、乙酸纤维素(例如,乙酸纤维素、三乙酸纤维素等)、赛璐玢、硅酮、聚氯乙烯(例如,聚偏二氯乙烯)、含氟聚合物(例如,聚氟乙烯、聚偏二氟乙烯、聚四氟乙烯和乙烯-四氟乙烯共聚物)以及它们两种或更多种的组合。所述聚合物膜可以是非取向的、单轴取向的或双轴取向的。可用于光伏电池模块外层(例如,入射层或背衬层)的膜的具体实例包括,但不限于,聚酯膜(例如,聚(对苯二甲酸乙二醇酯)膜)、含氟聚合物膜(例如,可从杜邦获得的和膜)。金属膜如铝箔也可用作背衬层。此外,用于所述太阳电池组件外层的膜可以是多层膜形式,如含氟聚合物/聚酯/含氟聚合物多层膜(例如,)或可从Austria的Isovolta AG或Woburn MA的Madico获得TPT层压膜。
在一种方法中,将光电池模块的组成层以期望的顺序堆叠以形成预层压组合件。然后,将所述组合件放置到能够维持真空的袋("真空袋"),通过真空管线或其它方法从所述袋抽出空气,密封所述袋同时保持真空(例如,至少约27-28in.Hg(689-711mm Hg),并将所述密封的袋放置到高压釜中,升高压力至约150psi至约250psi(约11.3巴至约18.8巴),温度为约135℃至约180℃,持续约10分钟至约50分钟。真空环可代替所述真空袋。美国专利第3,311,517号中描述了一种适合的真空袋。在热和压力循环后,冷却所述高压釜中的空气,但不添加额外的空气,以保持所述高压釜中的压力。在冷却约20分钟后,排出过量的空气压力,并从所述高压釜中移出所述层压体。或者,可在约80℃至约120℃的烘箱中加热所述预层压组合件约20分钟至约40分钟,然后,可使经加热的组合件通过一组夹压辊,以挤出各层之间空隙空间中的空气,再密封所述组合件的边缘。此阶段的组合件称为预压件。然后,可将所述预压件放置到温度升高到约135℃至约180℃且压力为约100psi至约300psi(约6.9巴至约20.7巴)的空气高压釜中。保持这些条件约15分钟至约60分钟,此后冷却空气,同时不再向所述高压釜引入空气。在冷却约20分钟至约40分钟后,排出过量的空气压力,并从所述高压釜中移出所述层压产品。光伏电池模块也可通过非高压釜法制备。这些非高压釜法描述在例如美国专利第3,234,062;3,852,136;4,341,576;4,385,951;4,398,979;5,536,347;5,853,516;6,342,116和5,415,909号;美国专利公开号2004/0182493;欧洲专利第1235683B1号和PCT专利公开号WO91/01880和WO03/057478中。通常,非高压釜法包括加热预层压组合件和施加真空、压力或这两者。例如,所述组合件可连续地通过加热烘箱和夹压辊。
在一个实施方式中,所述可固化封装剂膜适合作为用于光电子、OLED、光伏电池、有机光伏电池、柔性薄膜有机光伏电池、CIGS光伏电池等的封装剂。在一个优选的实施方式中,所述封装剂适合作为有机光伏电池(OPV)用的封装剂,其中最需要湿气和氧气阻隔要求。与常规液体封装剂相比,所述可固化封装剂膜具有许多优点。在此描述的可固化封装剂允许材料在层压过程中围绕光伏电池组合件的不规则表面和在其上面完全流动,因而将气泡和电池破裂减到最少。此外,引入PIB和完全相容的反应性(甲基)丙烯酸类官能化的PIB或聚烯烃低聚物/聚合物给予所述封装剂层高的湿气和氧气阻隔性以及光学透明度。
在一个实施方式中,与具有含有挥发性低分子量分子的封装剂层的电池相比,具有不含有挥发性低分子量(Mw小于约1,000Da)有机分子的封装剂层的有机光伏电池具有更高的模块效率。不希望受理论约束,相信此类分子存在于封装剂层中可能在加热时形成空隙,影响所述封装剂层与活性有机层之间的粘合性,更重要的是,由于所述活性有机层中低有机分子的迁移和溶剂化,改变所述活性有机层的形态。如从"Organic Photovoltaics:Challenges and Opportunities,"by Russell Gaudiana,J.of Polymer Science:PartB:Polymer Physics 2012,DOI:10.1002/polb.23083)可知,活性层的形态对模块效率至关重要。例如,高比例的加工时间集中在控制溶剂从活性有机组分的蒸发速率,因为其是形成活性层最优形态的主要因素。所述活性层的涂布质量可由尽可能的精密厚度、表面粗糙度和无针孔膜决定。
在另一个实施方式中,所述封装剂层的模量小于约50×104Pa(帕斯卡)。在一个实施方式中,所述封装剂层的模量在约1×104Pa至约5×104Pa、优选约1×104Pa至约3×104Pa的范围内。由于电子器件需要更高的柔软性,因而包括封装剂层的组件的较低模量是合乎需要的。
提供下述实施例以进一步详细描述本发明。这些实施例阐述目前预期进行本发明的优选方式,其意图是说明而不是限制本发明。
实施例
样品的组分如下。
均来自BASF的Oppanol PIB系列和Glassipol系列为PIB。
PIB二丙烯酸酯是Mw约为14,000的具有两个末端丙烯酸酯基的PIB。这是根据T.P.Liao和J.P.Kennedy,Polymer Bulletin,第6卷,135-141页(1981)中描述的方法合成的。
来自Sartomer的CN308为反应性聚丁二烯二丙烯酸酯。
来自Rextac LLC的RT2814和RT2315为190℃下的布氏粘度小于8,000cps的非结晶性聚α-烯烃。
来自Exxon Mobil的Linxar系列为半结晶性C2-C6聚烯烃,其Mw小于约100,000Da,多分散指数小于约3和熔点低于约100℃。
来自BASF的Irgacure系列和Lucirin TPO-L为光引发剂。
来自Arkema的Luperox系列为热引发剂。
来自Akzo Nobel的Trigonox 101为热引发剂。
来自Exxon Mobil的Escorez 5380为增粘剂。
来自Sartomer的SR833S为双官能的丙烯酸酯单体,其分子量为304Da。
按如下测定样品的粘度、水蒸气透过率(WVTR)、水吸收、透光百分率(%T)、折射指数、剪切强度、空隙形成和模量。
使用布鲁克费尔德粘度计,27转子,在80℃、120℃或130℃下,测定一些未固化的封装剂的粘度。此外,使用流变仪,通过10rad/s频率下的温度扫描,测定一些实施例的粘度。
通过使用ARES-M流变仪测定一些未固化的封装剂的粘度。
在18密耳厚的固化的封装剂膜上测定WVTR、水分吸收、光透射率和折射指数值。除非另作说明,否则使用实验室规模的热熔式涂布机(来自ChemInstruments的Hot MeltCoater HLC-101),在130℃下,在2密耳硅酮离型PET(聚对苯二甲酸乙二醇酯)衬垫上,以热熔体形式涂布所述封装剂。通过用D-bulb(Fusion Systems)以500-5000mJ/cm2(取决于样品)的UVA&B剂量照射,或通过在150-170℃(取决于样品)的烘箱中加热封装剂膜,固化所述封装剂膜。移除所述衬垫,并在18密耳厚的固化的封装剂膜上进行测试。
根据ASTM F-1249,在38℃/100%RH下,用Mocon Permeatran 3/33测定WVTR。
用Surface Measurement Systems,Ltd.的Dynamic Vapour Sorption DVS-2000测定水分吸收。
用Perkin Elmer UV/Vis光谱仪测定光透射率(%T)。
用ATAGO的ABBE Refractomer测定折射指数值。
根据PSTC-107,程序A测定固化的封装剂膜的剪切强度,修改如下:(1)如上所述在2密耳PET阻隔膜上涂布5-6密耳厚的封装剂,用2密耳PET离型衬垫层压,如上所述固化,然后在23℃和50%相对湿度下调节;(2)在浸湿不锈钢测试面板15分钟后,在12×25mm区域上,施加500g的剪切载荷,测定剪切粘合性。在23℃和50%相对湿度下进行剪切强度测试。
对于层压空隙测试,在如上的2密耳硅酮离型PET衬垫上,以约5-6密耳的厚度涂布封装剂。将封装剂膜从所述衬垫转移并在120℃下使用来自Western Magnum的XRL 180 HotRoll Laminator层压在两个PET阻隔膜之间,以促进在包含盖板和基板的器件上的粘合。如上所述固化封装剂膜。冷却之后,透过PET阻隔膜目视检查空隙(气泡)形成。
实施例1
样品1-6的组分列出在表1中。如本领域技术人员已知的,通过在Brabender中或用Glas-Col在130℃下混合所述组分来制备所有样品。对于样品2和5,冷却样品至80℃,然后添加热引发剂。样品4的布氏粘度曲线示出在图1中。
表1
然后,如上所述,将样品1-6的封装剂涂布成膜,并固化。在38℃/100%RH下,在18密耳厚的纯封装剂膜上测定WVTR。在18密耳厚的固化的封装剂膜上测定水吸收、%T、折射指数和剪切强度。
层压测试表明上述样品没有看得见的空隙。
实施例2
样品4和对比样品C-1至C-4的组分和性质列出在表2中。类似于实施例1中的样品,制备对比样品C-1至C-4。
表2
*粘度数据来自于流变仪。
添加低分子量SR833S在120℃下的层压期间没有不利地影响剪切强度或引起空隙,然而,使用由低分子量单体形成的封装剂膜会显著降低有机电子器件的性能,经常导致较低效率。
实施例3
将增粘剂添加到表3中列出的对比配制物C-5至C-8。类似于实施例1的样品,制备对比样品C-5至C-8。
表3
*粘度数据来自于流变仪。
对比样品的粘度随着增粘剂的添加而降低,然而,添加低分子量单体会降低有机电子器件的性能。
实施例4
样品7-12的组分列出在表4中。类似于实施例1,制备样品。
表4
*粘度数据来自于流变仪。
样品7-11具有在80℃下可接受的低粘度,因而可以热熔体形式且没有任何溶剂涂布或挤出,即使在低于100℃的温度下也可以。
除低温下的可涂布粘度之外,样品7、10和11的低模量值(模量值小于约10×104dyn/cm2)表明这些材料还是柔性和软胶状的,这对于一些电子显示器是希望的。
在不背离本发明的精神和范围的情况下,可对本发明进行许多修改和改变,这对本领域技术人员来说是显而易见的。在此描述的具体实施方式仅作为实例提供,本发明将仅受所附权利要求的各项以及与这些权利要求等同的全部范围限制。
Claims (20)
1.一种可固化封装剂,该可固化封装剂包含:
a)基于可固化封装剂的总重量,约70重量%至约90重量%的Mw为约1,000Da至约95,000Da的聚异丁烯;
b)基于可固化封装剂的总重量,约10重量%至约50重量%的官能化聚异丁烯,该官能化聚异丁烯具有(i)约1,000Da至约95,000Da的Mw和(ii)每个聚合物链多于一个的自由基反应性官能团,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯和/或末端丙烯酸酯组成的组;
c)自由基引发剂;和
d)UV吸收剂;
其中所述可固化封装剂(i)基本上不含Mw小于约1,000Da的丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物;和(ii)基本上不含增粘剂;且(iii)是热熔体。
2.权利要求1所述的可固化封装剂,其中,所述UV吸收剂选自由苯并三唑衍生物类、羟基二苯甲酮类、羟苯基三嗪类、取代的和未被取代的苯甲酸的酯、受阻胺光稳定剂以及它们的任意混合物组成的组。
3.权利要求2所述的可固化封装剂,其中,所述受阻胺光稳定剂是仲、叔、乙酰化、N-烃氧基取代的、羟基取代的N-烃氧基取代的或取代的环胺,其特征在于在与胺官能团邻近的碳原子上的脂肪族取代。
4.权利要求1所述的可固化封装剂,进一步包含官能化聚烯烃,所述官能化聚烯烃具有(i)约1,000Da至约95,000Da的Mw和(ii)多于一个的自由基反应性基团;
所述自由基反应性官能团选自由末端(甲基)丙烯酸酯和/或末端丙烯酸酯组成的组。
5.权利要求1所述的可固化封装剂,进一步包含至多20重量%的多种干燥剂填料。
6.权利要求1所述的可固化封装剂,其包含小于5,000ppm的Mw小于1,000Da的挥发性有机分子。
7.一种可固化封装剂,该可固化封装剂包含:
a)基于可固化封装剂的总重量,约70重量%至约90重量%的Mw为约1,000Da至约95,000Da的聚异丁烯;
b)基于可固化封装剂的总重量,约10重量%至约50重量%的官能化聚烯烃,该官能化聚烯烃具有(i)约1,000Da至约95,000Da的Mw和(ii)每个聚合物链多于一个的自由基反应性官能团,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯和/或末端丙烯酸酯组成的组;
c)自由基引发剂;和
d)UV吸收剂;
其中所述可固化封装剂(i)基本上不含Mw小于约1,000Da的丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物;和(ii)基本上不含增粘剂;且(iii)是热熔体。
8.权利要求7所述的可固化封装剂,其中,所述UV吸收剂选自由苯并三唑衍生物类、羟基二苯甲酮类、羟苯基三嗪类、取代的和未被取代的苯甲酸的酯、受阻胺光稳定剂以及它们的任意混合物组成的组。
9.权利要求7所述的可固化封装剂,其中,所述受阻胺光稳定剂是仲、叔、乙酰化、N-烃氧基取代的、羟基取代的N-烃氧基取代的或取代的环胺,其特征在于在与胺官能团邻近的碳原子上的脂肪族取代。
10.权利要求7所述的可固化封装剂,其中,所述官能化聚烯烃选自由(甲基)丙烯酸酯封端的聚丁二烯、氢化的(甲基)丙烯酸酯封端的聚丁二烯和它们的混合物组成的组。
11.权利要求7所述的可固化封装剂,进一步包含至多20重量%的多种干燥剂填料。
12.权利要求7所述的可固化封装剂,其包含小于5,000ppm的Mw小于1,000Da的挥发性有机分子。
13.一种可固化封装剂,该可固化封装剂包含:
a)基于可固化封装剂的总重量,约70重量%至约90重量%的在190℃下的布氏粘度小于8,000cps的非结晶性聚α烯烃;
b)基于可固化封装剂的总重量,约10重量%至约50重量%的官能化聚丁二烯和/或官能化聚烯烃,该官能化聚丁二烯和/或官能化聚烯烃具有(i)约1,000Da至约95,000Da的Mw和(ii)每个聚合物链多于一个的自由基反应性官能团,其中所述自由基反应性官能团选自由末端(甲基)丙烯酸酯和/或末端丙烯酸酯组成的组;
c)自由基引发剂;
d)增粘剂;和
e)UV吸收剂;
其中所述可固化封装剂(i)基本上不含Mw小于约1,000Da的丙烯酸类单体或Mw小于约1,000Da的挥发性有机化合物;和(ii)是热熔体。
14.权利要求13所述的可固化封装剂,其中,所述UV吸收剂选自由苯并三唑衍生物类、羟基二苯甲酮类、羟苯基三嗪类、取代的和未被取代的苯甲酸的酯、受阻胺光稳定剂以及它们的任意混合物组成的组。
15.权利要求13所述的可固化封装剂,其中,所述受阻胺光稳定剂是仲、叔、乙酰化、N-烃氧基取代的、羟基取代的N-烃氧基取代的或取代的环胺,其特征在于在与胺官能团邻近的碳原子上的脂肪族取代。
16.权利要求13所述的可固化封装剂,其中,所述官能化聚烯烃选自由(甲基)丙烯酸酯封端的聚丁二烯、氢化的(甲基)丙烯酸酯封端的聚丁二烯和它们的混合物组成的组。
17.权利要求13所述的可固化封装剂,进一步包含至多20重量%的多种干燥剂填料。
18.包含权利要求1所述的可固化封装剂的制品,所述制品为电子器件。
19.包含权利要求7所述的可固化封装剂的制品,所述制品为电子器件。
20.包含权利要求13所述的可固化封装剂的制品,所述制品为电子器件。
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US9676928B2 (en) | 2017-06-13 |
KR20150008873A (ko) | 2015-01-23 |
CN104584257B (zh) | 2017-06-20 |
KR20180087470A (ko) | 2018-08-01 |
JP6423339B2 (ja) | 2018-11-14 |
US10141532B2 (en) | 2018-11-27 |
JP2015528023A (ja) | 2015-09-24 |
TW201402740A (zh) | 2014-01-16 |
US20170244058A1 (en) | 2017-08-24 |
EP2845241A4 (en) | 2016-02-10 |
EP2845241A1 (en) | 2015-03-11 |
CN104584257A (zh) | 2015-04-29 |
KR101919294B1 (ko) | 2018-11-15 |
TWI623598B (zh) | 2018-05-11 |
US20150056757A1 (en) | 2015-02-26 |
WO2013165637A1 (en) | 2013-11-07 |
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