CN109863180B - 伸缩性树脂层形成用固化性组合物 - Google Patents
伸缩性树脂层形成用固化性组合物 Download PDFInfo
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- CN109863180B CN109863180B CN201780066013.0A CN201780066013A CN109863180B CN 109863180 B CN109863180 B CN 109863180B CN 201780066013 A CN201780066013 A CN 201780066013A CN 109863180 B CN109863180 B CN 109863180B
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Images
Classifications
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Abstract
本发明公开一种伸缩性树脂层形成用固化性组合物,其含有:(A)具有聚苯乙烯链的弹性体;(B)单官能的直链烷基(甲基)丙烯酸酯;(C)具有脂环基的单官能的(甲基)丙烯酸酯;(D)具有2个以上的烯属不饱和基的2官能以上的化合物;及(E)聚合引发剂。
Description
技术领域
本发明涉及形成伸缩性树脂层的固化性组合物、及具有伸缩性树脂层的半导体装置。
背景技术
近年来,对可穿戴设备的需求越来越高。对于可穿戴设备,除了要求小型化以外,还要求具有柔性及伸缩性,以便易于穿戴到身体的曲面及抑制与移除相伴随的连接不良。要求柔性及伸缩性的构件通常可以利用液状硅酮或液状聚氨酯来形成。
专利文献1公开了一种含有苯乙烯系弹性体的挠性树脂层形成用树脂组合物。
专利文献2公开了一种含有共聚物橡胶的耐热性防湿绝缘涂料,所述共聚物橡胶含有聚苯乙烯链的嵌段。专利文献3公开了一种光固化性树脂组合物,其含有具有烯属不饱和双键的氨基甲酸酯化合物及具有环状脂肪侧基的光聚合性单体。
现有技术文献
专利文献
专利文献1:国际公开第2016/080346号
专利文献2:日本特开2005-162986号公报
专利文献3:日本特开2007-308681号公报
发明内容
发明要解决的课题
例如,期待对搭载于可穿戴设备的半导体元件进行密封的密封树脂层具有高的伸缩性。另外,还需要与构成可穿戴设备等的柔性基材之类的伸缩性基材具有充分的密合性的伸缩性树脂层。
因此,本发明的一方面的目的在于,提供可以形成具有充分的伸缩性及密合性的伸缩性树脂层的固化性组合物。
用于解决课题的手段
本发明的一方面提供一种伸缩性树脂层形成用固化性组合物,其含有:(A)具有聚苯乙烯链的弹性体;(B)单官能的直链烷基(甲基)丙烯酸酯;(C)具有脂环基的单官能的(甲基)丙烯酸酯;(D)具有2个以上的烯属不饱和基的2官能以上的化合物;及(E)聚合引发剂。换言之,本发明的一方面涉及上述固化性组合物的在制造伸缩性树脂层上的应用或使用。
本发明人们反复进行了深入研究,结果发现,含有上述特定的成分的组合的固化性组合物可以形成具有充分的伸缩性及密合性的伸缩性树脂层。
发明效果
本发明的一方面的固化性组合物可以形成具有充分的伸缩性及密合性的伸缩性树脂层。
附图说明
图1是示出伸缩恢复率的测定例的应力-应变曲线。
图2是示出半导体装置的一实施方式的剖视图。
图3是示出挠性基板及电路部件的一实施方式的剖视图。
图4是示出得到多个半导体装置的工序的一实施方式的剖视图。
具体实施方式
以下对本发明的几个实施方式进行详细说明。但是,本发明不受以下的实施方式限定。
[固化性组合物]
一实施方式的固化性组合物含有:(A)具有聚苯乙烯链的弹性体;(B)单官能的直链烷基(甲基)丙烯酸酯;(C)具有脂环基的单官能的(甲基)丙烯酸酯;(D)具有2个以上的烯属不饱和基的2官能以上的化合物;及(E)聚合引发剂。该固化性组合物可以通过照射活性光线或加热来固化,从而形成具有伸缩性的固化物或固化膜。
本说明书中,“伸缩性”是指:在利用拉伸载荷产生应变后,能够通过解除载荷而恢复到原形状或接近原形状的性质。例如,在利用拉伸载荷产生50%的应变后,能够恢复到原形状或接近原形状的材料可以称之为具有伸缩性。更具体而言,后述的伸缩恢复率为80%以上的树脂层可以称之为伸缩性树脂层。
(A)弹性体
具有聚苯乙烯链的弹性体(以下有时称为“苯乙烯系弹性体”。)例如可以是:具有作为硬链段的聚苯乙烯链、和作为软链段的聚二烯链(例如聚丁二烯链、聚异戊二烯链)的共聚物。作为这类苯乙烯系弹性体的市售品,可列举例如JSR(株)“Dynaron SEBS系列”、Kraton Polymers Japan(株)“Kraton D聚合物系列”、Aron化成(株)“AR系列”。
苯乙烯系弹性体的聚二烯链的双键可以通过氢化而实现饱和。具有经氢化的聚丁二烯链的苯乙烯系弹性体可以是苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(氢化型苯乙烯丁二烯共聚聚合物)。具有经过氢化的聚异戊二烯链的苯乙烯系弹性体可以是苯乙烯-乙烯/丙烯-苯乙烯嵌段共聚物(氢化苯乙烯异戊二烯共聚聚合物)。认为具有经过氢化的聚二烯链的苯乙烯系弹性体有助于提高耐候性。作为具有经过氢化的聚二烯链的苯乙烯系弹性体的市售品,可列举例如JSR(株)“Dynaron HSBR系列”、Kraton Polymers Japan(株)“Kraton G聚合物系列”、旭化成(株)“Tuftec系列”、(株)可乐丽“SEPTON系列”。
从固化性组合物的涂敷性的观点出发,苯乙烯系弹性体的重均分子量可以为30000~200000或50000~150000。在此,重均分子量(Mw)是指:利用凝胶渗透色谱(GPC)求出的标准聚苯乙烯换算值。
(A)成分的苯乙烯系弹性体的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量可以为10~50质量%或20~40质量%。当苯乙烯系弹性体的含量为10质量%以上时,有容易提高伸缩性的倾向。当苯乙烯系弹性体的含量为50质量%以下时,固化性组合物的粘度降低,因此有涂敷性提高的倾向。
(B)单官能的直链烷基(甲基)丙烯酸酯
单官能的直链烷基(甲基)丙烯酸酯为具有1个(甲基)丙烯酰基及直链烷基的酯化合物。通常,单官能的直链烷基(甲基)丙烯酸酯为由(甲基)丙烯酸与直链烷基醇形成的酯化合物。直链烷基(甲基)丙烯酸酯所具有的直链烷基的碳数可以为12以下或10以下。当该碳数为12以下时,特别是在使用具有经过氢化的聚二烯链的弹性体时,存在由固化性组合物形成的固化物不易发生白浊的倾向。直链烷基的碳数可以为6以上或8以上。
作为单官能的直链烷基(甲基)丙烯酸酯的例子,可列举:(甲基)丙烯酸异辛酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸月桂酯、丙烯酸异硬脂酯、丙烯酸硬脂酯及丙烯酸十三烷基酯。这些中,可以选择:选自具有碳数12以下的直链烷基的(甲基)丙烯酸异辛酯、(甲基)丙烯酸异癸酯及(甲基)丙烯酸月桂酯中的一种以上化合物。这些化合物可以单独使用或将两种以上组合使用,也可以将这些化合物与其它的单官能的直链烷基(甲基)丙烯酸酯组合。
(B)成分的单官能的直链烷基(甲基)丙烯酸酯的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量可以为10~50质量%或20~40质量%。当(B)成分的含量为10质量%以上时,有伸缩性提高的效果相对增大的倾向。当(B)成分的含量为50质量%以下时,有密合性提高的效果相对提高的倾向。
(C)具有脂环基的单官能的(甲基)丙烯酸酯
具有脂环基的单官能的(甲基)丙烯酸酯通常为由(甲基)丙烯酸与具有脂环基的醇化合物形成的酯化合物。具有脂环基的单官能的(甲基)丙烯酸酯例如可以为选自丙烯酸环己酯、(甲基)丙烯酸3,3,5-三甲基环己酯、(甲基)丙烯酸4-叔丁基环己酯、丙烯酸异冰片酯、丙烯酸二环戊酯(丙烯酸三环癸酯)及丙烯酸四氢糠酯中的一种以上化合物。这些化合物可以单独使用或将两种以上组合使用,也可以将这些化合物与其它具有脂环基的单官能的(甲基)丙烯酸酯组合。
(C)成分的具有脂环基的单官能的(甲基)丙烯酸酯的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量可以为10~50质量%或20~40质量%。当(C)成分的含量为10质量%以上时,有密合性提高的效果相对提高的倾向。当(C)成分的含量为50质量%以下时,有伸缩性提高的效果相对提高的倾向。
(D)具有2个以上的烯属不饱和基的2官能以上的化合物
具有2个以上的烯属不饱和基的2官能以上的化合物所具有的烯属不饱和基例如可以为(甲基)丙烯酰基、乙烯基或它们的组合。作为具有2个以上的烯属不饱和基的2官能以上的化合物,可列举例如:(甲基)丙烯酸酯、偏二卤乙烯、乙烯基醚、乙烯基酯、乙烯基吡啶、乙烯基酰胺、芳基化乙烯基(日文:アリール化ビニル)。这些中,从伸缩性树脂层的透明性的观点出发,可以选择(甲基)丙烯酸酯或芳基化乙烯基中的至少一者。
作为具有2个(甲基)丙烯酰基的2官能(甲基)丙烯酸酯,可列举例如:乙二醇二(甲基)丙烯酸酯、二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、二丙二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、四丙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、乙氧基化聚丙二醇二(甲基)丙烯酸酯、1,3-丁二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、3-甲基-1,5-戊二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、2-丁基-2-乙基-1,3-丙二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,10-癸二醇二(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、三环癸烷二甲醇二(甲基)丙烯酸酯及乙氧基化2-甲基-1,3-丙二醇二(甲基)丙烯酸酯等脂肪族(甲基)丙烯酸酯;环己烷二甲醇二(甲基)丙烯酸酯、乙氧基化环己烷二甲醇二(甲基)丙烯酸酯、丙氧基化环己烷二甲醇二(甲基)丙烯酸酯、乙氧基化丙氧基化环己烷二甲醇二(甲基)丙烯酸酯、三环癸烷二甲醇二(甲基)丙烯酸酯、乙氧基化三环癸烷二甲醇二(甲基)丙烯酸酯、丙氧基化三环癸烷二甲醇二(甲基)丙烯酸酯、乙氧基化丙氧基化三环癸烷二甲醇二(甲基)丙烯酸酯、乙氧基化氢化双酚A二(甲基)丙烯酸酯、丙氧基化氢化双酚A二(甲基)丙烯酸酯、乙氧基化丙氧基化氢化双酚A二(甲基)丙烯酸酯、乙氧基化氢化双酚F二(甲基)丙烯酸酯、丙氧基化氢化双酚F二(甲基)丙烯酸酯及乙氧基化丙氧基化氢化双酚F二(甲基)丙烯酸酯等脂环式(甲基)丙烯酸酯;乙氧基化双酚A二(甲基)丙烯酸酯、丙氧基化双酚A二(甲基)丙烯酸酯、乙氧基化丙氧基化双酚A二(甲基)丙烯酸酯、乙氧基化双酚F二(甲基)丙烯酸酯、丙氧基化双酚F二(甲基)丙烯酸酯、乙氧基化丙氧基化双酚F二(甲基)丙烯酸酯、乙氧基化双酚AF二(甲基)丙烯酸酯、丙氧基化双酚AF二(甲基)丙烯酸酯、乙氧基化丙氧基化双酚AF二(甲基)丙烯酸酯、乙氧基化芴型二(甲基)丙烯酸酯、丙氧基化芴型二(甲基)丙烯酸酯及乙氧基化丙氧基化芴型二(甲基)丙烯酸酯等芳香族(甲基)丙烯酸酯;乙氧基化异氰脲酸二(甲基)丙烯酸酯、丙氧基化异氰脲酸二(甲基)丙烯酸酯及乙氧基化丙氧基化异氰脲酸二(甲基)丙烯酸酯等杂环式(甲基)丙烯酸酯;它们的己内酯改性体;新戊二醇型环氧(甲基)丙烯酸酯等脂肪族环氧(甲基)丙烯酸酯;环己烷二甲醇型环氧(甲基)丙烯酸酯、氢化双酚A型环氧(甲基)丙烯酸酯及氢化双酚F型环氧(甲基)丙烯酸酯等脂环式环氧(甲基)丙烯酸酯;以及间苯二酚型环氧(甲基)丙烯酸酯、双酚A型环氧(甲基)丙烯酸酯、双酚F型环氧(甲基)丙烯酸酯、双酚AF型环氧(甲基)丙烯酸酯及芴型环氧(甲基)丙烯酸酯等芳香族环氧(甲基)丙烯酸酯。
作为具有3个以上的(甲基)丙烯酰基的3官能以上的多官能(甲基)丙烯酸酯,可列举例如:三羟甲基丙烷三(甲基)丙烯酸酯、乙氧基化三羟甲基丙烷三(甲基)丙烯酸酯、丙氧基化三羟甲基丙烷三(甲基)丙烯酸酯、乙氧基化丙氧基化三羟甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、乙氧基化季戊四醇三(甲基)丙烯酸酯、丙氧基化季戊四醇三(甲基)丙烯酸酯、乙氧基化丙氧基化季戊四醇三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、乙氧基化季戊四醇四(甲基)丙烯酸酯、丙氧基化季戊四醇四(甲基)丙烯酸酯、乙氧基化丙氧基化季戊四醇四(甲基)丙烯酸酯、二(三羟甲基丙烷)四丙烯酸酯及二季戊四醇六(甲基)丙烯酸酯等脂肪族(甲基)丙烯酸酯;乙氧基化异氰脲酸三(甲基)丙烯酸酯、丙氧基化异氰脲酸三(甲基)丙烯酸酯及乙氧基化丙氧基化异氰脲酸三(甲基)丙烯酸酯等杂环式(甲基)丙烯酸酯;它们的己内酯改性体;以及苯酚酚醛型环氧(甲基)丙烯酸酯及甲酚酚醛型环氧(甲基)丙烯酸酯等芳香族环氧(甲基)丙烯酸酯。
从与苯乙烯系弹性体的相容性、透明性、耐热性、对聚酰亚胺及铜箔的密合性的观点出发,(D)成分可以为具有脂环基的化合物;作为其例子,可列举环己烷二甲醇二(甲基)丙烯酸酯、及三环癸烷二甲醇二(甲基)丙烯酸酯。
以上例示的化合物可以单独使用或将两种以上组合使用,也可以将所选择的化合物与其它的2官能以上的化合物组合。
(D)成分的2官能以上的化合物的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量可以为0.3~20质量%、0.5~10质量%或1~5质量%。当(D)成分的含量为0.3质量%以上时,有在固化后粘性降低的倾向、及伸缩性提高的效果相对提高的倾向。当(D)成分的含量为20质量%以下时,有伸缩性提高的效果相对提高的倾向。
(E)聚合引发剂
聚合引发剂是通过加热或照射紫外线等来引发聚合的化合物,例如可以为热自由基聚合引发剂或光自由基聚合引发剂。从固化速度快、能常温固化的角度出发,可以选择光自由基聚合引发剂。
作为热自由基聚合引发剂,可列举例如:过氧化甲乙酮、过氧化环己酮及过氧化甲基环己酮等酮过氧化物;1,1-双(叔丁基过氧化)环己烷、1,1-双(叔丁基过氧化)-2-甲基环己烷、1,1-双(叔丁基过氧化)-3,3,5-三甲基环己烷、1,1-双(叔己基过氧化)环己烷及1,1-双(叔己基过氧化)-3,3,5-三甲基环己烷等过氧化缩酮;过氧化氢对孟烷等氢过氧化物;α,α’-双(叔丁基过氧化)二异丙基苯、二枯基过氧化物、叔丁基枯基过氧化物及二叔丁基过氧化物等二烷基过氧化物;过氧化辛酰、过氧化月桂酰、过氧化硬脂酰及过氧化苯甲酰等二酰基过氧化物;过氧化二碳酸双(4-叔丁基环己基)酯、过氧化二碳酸二-2-乙氧基乙酯、过氧化二碳酸二-2-乙基己酯及过氧化碳酸二-3-甲氧基丁酯等过氧化碳酸酯;过氧化新戊酸叔丁酯、过氧化新戊酸叔己酯、过氧化-2-乙基己酸1,1,3,3-四甲基丁酯、2,5-二甲基-2,5-双(2-乙基己酰基过氧化)己烷、过氧化-2-乙基己酸叔己酯、过氧化-2-乙基己酸叔丁酯、过氧化异丁酸叔丁酯、过氧化异丙基单碳酸叔己酯、过氧化-3,5,5-三甲基己酸叔丁酯、过氧化月桂酸叔丁酯、过氧化异丙基单碳酸叔丁酯、过氧化-2-乙基己基单碳酸叔丁酯、过氧化苯甲酸叔丁酯、过氧化苯甲酸叔己酯、2,5-二甲基-2,5-双(苯甲酰基过氧化)己烷、过氧化乙酸叔丁酯等过氧化酯;以及2,2’-偶氮二异丁腈、2,2’-偶氮双(2,4-二甲基戊腈)及2,2’-偶氮双(4-甲氧基-2’-二甲基戊腈)等偶氮化合物。从固化性、透明性及耐热性的观点出发,热自由基聚合引发剂可以是上述二酰基过氧化物、上述过氧化酯、上述偶氮化合物或它们的组合。
作为光自由基聚合引发剂,可列举例如:2,2-二甲氧基-1,2-二苯基乙烷-1-酮等苯偶姻缩酮;1-羟基环己基苯基酮、2-羟基-2-甲基-1-苯基丙烷-1-酮及1-[4-(2-羟基乙氧基)苯基]-2-羟基-2-甲基-1-丙烷-1-酮等α-羟基酮;2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)-丁烷-1-酮及1,2-甲基-1-[4-(甲硫基)苯基]-2-吗啉代丙烷-1-酮等α-氨基酮;1-[(4-苯硫基)苯基]-1,2-辛二酮-2-(苯甲酰基)肟等肟酯;双(2,4,6-三甲基苯甲酰基)苯基氧化膦、双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦及2,4,6-三甲基苯甲酰基二苯基氧化膦等氧化膦;2-(邻氯苯基)-4,5-二苯基咪唑二聚物、2-(邻氯苯基)-4,5-二(甲氧基苯基)咪唑二聚物、2-(邻氟苯基)-4,5-二苯基咪唑二聚物、2-(邻甲氧基苯基)-4,5-二苯基咪唑二聚物及2-(对甲氧基苯基)-4,5-二苯基咪唑二聚物等2,4,5-三芳基咪唑二聚物;二苯甲酮、N,N,N’,N’-四甲基-4,4’-二氨基二苯甲酮、N,N,N’,N’-四乙基-4,4’-二氨基二苯甲酮及4-甲氧基-4’-二甲基氨基二苯甲酮等二苯甲酮化合物;2-乙基蒽醌、菲醌、2-叔丁基蒽醌、八甲基蒽醌、1,2-苯并蒽醌、2,3-苯并蒽醌、2-苯基蒽醌、2,3-二苯基蒽醌、1-氯蒽醌、2-甲基蒽醌、1,4-萘醌、9,10-菲醌、2-甲基-1,4-萘醌及2,3-二甲基蒽醌等醌化合物;苯偶姻甲醚、苯偶姻***及苯偶姻苯醚等苯偶姻醚;苯偶姻、甲基苯偶姻及乙基苯偶姻等苯偶姻化合物;苯偶酰二甲基缩酮等苯偶酰化合物;9-苯基吖啶、1,7-双(9,9’-吖啶基庚烷)等吖啶化合物;N-苯基甘氨酸;以及香豆素等。
在2,4,5-三芳基咪唑二聚物中,2个三芳基咪唑部位的芳基的取代基可以相同而提供对称的化合物,也可以不同而提供非对称的化合物。也可以如二乙基噻吨酮与二甲基氨基苯甲酸的组合那样将噻吨酮化合物与叔胺组合。
从固化性、透明性及耐热性的观点出发,光自由基聚合引发剂可以为上述α-羟基酮、上述氧化膦或它们的组合。这些热及光自由基聚合引发剂可以单独使用或将两种以上组合使用。也可以将这些与合适的敏化剂组合。
(E)成分的聚合引发剂的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量100质量份可以为0.1~10质量份、0.3~7质量份或0.5~5质量份。当(E)成分的含量为0.1质量份以上时,容易充分地进行固化。当(E)成分的含量为10质量份以下时,有透光性提高的倾向。
既可以直接使用液状或固态的固化性组合物,也可以将固化性组合物用有机溶剂稀释而制成树脂清漆。室温(25℃)下为液状的无溶剂的固化性组合物在没有有机溶剂的排出方面、可以容易地涂布于局部部分的方面等上有利。
有机溶剂可以从可溶解固化性组合物的各成分的有机溶剂中选择。作为有机溶剂,可列举例如:甲苯、二甲苯、均三甲苯、异丙苯及对异丙基甲苯等芳香族烃;四氢呋喃及1,4-二噁烷等环状醚;丙酮、甲基乙基酮、甲基异丁基酮、环己酮及4-羟基-4-甲基-2-戊酮等酮;乙酸甲酯、乙酸乙酯、乙酸丁酯、乳酸甲酯、乳酸乙酯及γ-丁内酯等酯;碳酸亚乙酯及碳酸亚丙酯等碳酸酯;N,N-二甲基甲酰胺、N,N-二甲基乙酰胺及N-甲基-2-吡咯烷酮等酰胺。从溶解性及沸点的观点出发,有机溶剂可以为甲苯、N,N-二甲基乙酰胺或它们的组合。这些有机溶剂可以单独使用或将两种以上组合使用。
固化性组合物可以根据需要而在含有以上说明的成分的基础上,还含有其它成分。作为其它成分,可列举例如:抗氧化剂、黄变防止剂、紫外线吸收剂、可见光吸收剂、着色剂、增塑剂、稳定剂、填充剂之类的添加剂。(A)成分、(B)成分、(C)成分及(D)成分的合计的含量在固化性组合物中相对于有机溶剂以外的成分的总量可以为例如85质量%以上、90质量%以上或95质量%以上。
[固化物(伸缩性树脂层)]
由固化性组合物形成的固化物(伸缩性树脂层)的弹性模量可以为0.1MPa以上且100MPa以下、0.2MPa以上且50MPa以下、或0.3MPa以上且30MPa以下。当固化物的弹性模量为0.1MPa以上时,有不易产生固化物彼此由于粘连而贴附的问题的倾向。当固化物的弹性模量为100MPa以下时,柔软性及伸缩性提高的效果可相对地提高。
由固化性组合物形成的固化物(伸缩性树脂层)的基于拉伸试验的断裂伸长率可以为100%以上。当固化物的断裂伸长率为100%以上时,可以得到更加优异的伸缩性。从同样的观点出发,固化物的断裂伸长率可以为150%以上或200%以上。
由固化性组合物形成的固化物(伸缩性树脂层)可以具有高的伸缩性。关于伸缩性,可以将通过含有2次拉伸试验的以下步骤而测定的、伸缩恢复性作为指标来进行评价。
1)准备长70mm、宽5mm的长条状的固化物作为试验片。
2)在用夹头间距离为50mm的夹头保持试验片的状态下,通过第1次拉伸试验将试验片拉伸至位移量(应变)X。
3)使夹头回到初始位置。
4)进行第2次拉伸试验,记录开始受到载荷的位置(载荷上升的位置)的位移量(应变)与X之差Y。
5)通过式:伸缩恢复率R=(Y/X)×100来计算伸缩恢复率。
拉伸试验在25℃的环境下进行。X可以设定为位移量25mm(应变50%)。作为试验机,可以使用例如Microforce试验机(Illinois Tool Works Inc、“Instron 5948”)。图1为由用于求出伸缩恢复性的拉伸试验得到的应力-应变曲线的例子。用于评价伸缩恢复性的试验片的厚度可以为100±10μm。
从耐受重复使用的观点出发,上述伸缩恢复率可以为80%以上、85%以上或90%以上。伸缩恢复率的上限没有特别限制,可以为100%。上述实施方式的固化性组合物通常可以容易地形成显示出80%的伸缩恢复率的固化物。
从透明性的观点出发,由固化性组合物形成的固化物(伸缩性树脂层)可以具有80%以上的总透光率、5.0以下的黄色指数(Yellowness Index,YI)及5.0%以下的雾度。总透光率、YI及雾度可以使用分光雾度计(日本电色工业(株)制、分光雾度计“SH7000”)来测定。可以是总透光率为85%以上、YI为4.0以下、雾度为4.0%以下。也可以是总透光率为90%以上、YI为3.0以下、雾度为3.0%以下。
由固化性组合物形成的固化物(伸缩性树脂层)例如可以作为构成可穿戴设备的伸缩性的密封树脂层来应用或使用。
[半导体装置]
图2是示意性示出一实施方式的半导体装置的剖视图。本实施方式的半导体装置100具备电路基板,所述电路基板由具有伸缩性的挠性基板1、电路部件2和伸缩性树脂层3构成。挠性基板1可以是伸缩性树脂层。电路部件2安装在挠性基板1上。伸缩性树脂层3可以为由上述实施方式的固化性组合物形成的固化物(固化膜)。伸缩性树脂层3通过使成膜后的固化性组合物固化来形成。伸缩性树脂层3将挠性基板1及电路部件2密封,保护电路基板的表面。
挠性基板1的构成材料可根据目的来选择。挠性基板1的构成材料可以为选自聚酰亚胺树脂、丙烯酸类树脂、硅树脂、氨基甲酸酯树脂、双马来酰亚胺树脂、环氧树脂及聚乙二醇树脂中的至少一种。其中,从伸缩性更优异的观点出发,挠性基板1的构成材料可以为选自具有硅氧烷结构、脂肪族醚结构或二烯结构的聚酰亚胺树脂、丙烯酸类树脂、硅树脂、氨基甲酸酯树脂、具有长链烷基链(例如碳数1~20的烷基链)的双马来酰亚胺树脂、环氧树脂、及具有轮烷结构的聚乙二醇树脂中的至少一种。进一步地,从伸缩性更优异的观点出发,挠性基板1的构成材料可以为选自具有硅氧烷结构或脂肪族醚结构或二烯结构的聚酰亚胺树脂、硅树脂、氨基甲酸酯树脂、及具有长链烷基链的双马来酰亚胺树脂中的至少一种。作为挠性基板1的构成材料,可以将选自这些树脂中的一种单独使用、或将两种以上组合使用。
电路部件2为例如存储器芯片、发光二极管(LED)、射频识别标签(RFID)、温度传感器、加速度传感器等安装部件。在1个挠性基板1上既可以安装一种电路部件,也可以混合安装两种以上的电路部件。在1个挠性基板1上可以安装1个或两个以上的电路部件2。
以下说明本实施方式的半导体装置的制造方法。
(工序1:安装工序)
首先,如图3所示,在挠性基板1上安装电路部件2。
(工序2:密封工序)
接下来,将挠性基板1及电路部件2用作为密封构件的固化性组合物密封。挠性基板1及电路部件2例如可以通过如下方式进行密封:将密封构件层叠于挠性基板1;将密封构件印刷在挠性基板1;或将挠性基板1浸渍于密封构件并进行干燥。密封可以通过印刷法、点胶机法、浸渍法等来进行。其中,在卷对卷(Roll to Roll)工艺中可以使用的方法可缩短制造工序。
(工序3:固化工序)
在密封工序中将挠性基板1及电路部件2用密封构件密封后,使密封构件(固化性组合物)固化,由此形成伸缩性树脂层3,得到具有伸缩性树脂层3的电路基板。由此,得到图1所示的半导体装置100。固化可以为利用加热的热固化、或利用曝光的光固化。
(工序4:切割工序)
半导体装置的制造方法根据需要可具备如下工序:例如,如图4所示,将电路基板切断、分离,由此得到具有电路部件的两个以上的半导体装置。由此,能够一次性、大面积地制造两个以上的半导体装置,减少制造工序这一点变得容易。
实施例
以下列举实施例进一步具体地说明本发明。但是,本发明不受这些实施例限定。
1.树脂清漆(固化性组合物)的制备
实施例1
将作为(A)成分的氢化苯乙烯异戊二烯共聚聚合物((株)可乐丽制“SEPTON2002”)30质量份、作为(B)成分的丙烯酸异癸酯(Arkema(株)制“Sartomer SR395”)30质量份、作为(C)成分的丙烯酸4-叔丁基环己酯(Arkema(株)制“Sartomer SR217”)37质量份、作为(D)成分的三环癸烷二甲醇二丙烯酸酯(新中村化学工业(株)制“NK Ester A-DCP”)2质量份、及作为(E)成分的双(2,4,6-三甲基苯甲酰基)苯基氧化膦(BASF公司制“Irgacure819”)1质量份在500ml烧瓶内在60℃下边搅拌边混合,得到树脂清漆。
实施例2~10及比较例1~3
按照表1所示的配合比(质量份)与实施例1同样地得到树脂清漆。
2.评价
[弹性模量、伸长率]
用刮刀涂布机((株)康井精机制“SNC-350”)将各实施例、比较例的树脂清漆涂布在表面脱模处理PET膜(Teijin DuPont Film(株)制“Purex A31”、厚25μm)的脱模处理面。利用紫外线曝光机(MIKASA(株)制“ML-320FSAT”)对树脂清漆的涂膜以2000mJ/cm2的曝光量照射紫外线(波长365nm),由此形成物性评价用的固化膜(伸缩性树脂层、厚度100μm)。
从固化膜切出长40mm、宽10mm的长条状的试验片。在25℃的环境下使用自动绘图仪((株)岛津制作所制“EZ-S”)进行该试验片的拉伸试验。由得到的应力-应变曲线求出固化膜的弹性模量及伸长率。拉伸试验在夹头间距离20mm、拉伸速度50mm/min的条件下进行。弹性模量由载荷0.5~1.0N的范围内的应力-应变曲线的斜率求出。伸长率由固化膜断裂时刻的应变(断裂伸长率)求出。
[伸缩恢复率]
从上述评价用的固化膜切出长70mm、宽5mm的长条状试验片。在25℃的环境下,通过使用了Microforce试验机(Illinois Tool Works Inc、“Instron 5948”)的2次拉伸试验来测定该试验片的恢复率。通过第1次拉伸试验将试验片拉伸到位移量(应变)X,然后,使夹头回到初始位置,进行第2次拉伸试验。在第2次拉伸试验中,在将开始受到载荷的位置(载荷上升的位置)的位移量(应变)与X之差设为Y时,伸缩恢复率R为由式:R=(Y/X)×100计算出的值。在该测定中,将初始长度(夹头间的距离)设为50mm、将X设为25mm(应变50%)。
[总透光率、YI、雾度]
从上述评价用的固化膜切出长30mm、宽30mm的试验片。在25℃的环境下用分光雾度计(日本电色工业(株)“SH7000”)测定该试验片的总透光率、YI及雾度。
[密合性的评价]
用刮刀涂布机((株)康井精机制“SNC-350”)将树脂清漆涂布于厚度50μm的聚酰亚胺膜(东丽杜邦(株)制“Kapton 100H”)上。利用紫外线曝光机(MIKASA(株)“ML-320FSAT”)以2000mJ/cm2的曝光量对树脂清漆的涂膜照射紫外线(波长365nm),从而在聚酰亚胺膜上形成固化膜(伸缩性树脂层、厚度100μm)。从聚酰亚胺膜与固化膜的层叠体切出长50mm、宽10mm的长条状的试验片。将该试验片的固化膜侧用粘接剂(Cemedine(株)制“Cemedine Super-x Gold”固定在铜板上。在25℃的环境下,用自动绘图仪((株)岛津制作所“EZ-S”)以50mm/min的速度沿着与固化膜成90度角的方向从固定于铜板的固化膜剥离聚酰亚胺膜。基于此时每单位宽度的拉伸应力(N/cm)的最大值评价密合性。
[表1]
(A)弹性体
1)SEPTON 2002(氢化苯乙烯异戊二烯共聚聚合物、(株)可乐丽、重均分子量:55,000)
2)Kraton MD6951(氢化型苯乙烯丁二烯共聚聚合物、Kraton Polymers Japan(株)、重均分子量:60,000)
3)KAYAFLEX BPAM-155(橡胶改性聚酰胺、日本化药(株)、重均分子量:31,000)
(B)单官能的直链烷基(甲基)丙烯酸酯
4)SR395(丙烯酸异癸酯、Arkema(株)、“Sartomer SR395”)
5)SR440(丙烯酸异辛酯、Arkema(株)、“Sartomer SR440”)
6)LA(丙烯酸月桂酯、大阪有机化学工业(株))
(C)具有脂环式基团的单官能的(甲基)丙烯酸酯
7)SR217(丙烯酸4-叔丁基环己酯、Arkema(株)、“Sartomer SR217”)
8)SR420(丙烯酸3,3,5-三甲基环己酯(Arkema(株)、“Sartomer SR420”)
9)FA-513AS(丙烯酸二环戊酯、日立化成(株)、“Fancryl FA-513AS”)
10)Blemmer CHA(丙烯酸环己酯、日油(株))
(D)2官能以上的化合物
11)A-DCP(三环癸烷二甲醇二丙烯酸酯、新中村化学工业(株)、“NK Ester A-DCP”)
12)CD406(环己烷二甲醇二丙烯酸酯、Arkema(株)、“Sartomer CD406”)
13)FA-129AS(壬二醇二丙烯酸酯(日立化成(株)、“Fancryl FA-129AS”)
(E)聚合引发剂
14)Irgacure819(双(2,4,6-三甲基苯甲酰基)苯基氧化膦、BASF JAPAN(株))
表1示出评价结果。由各实施例的树脂清漆(固化性组合物)形成的固化膜(伸缩性树脂层)显示出充分优异的伸缩性及密合性。另一方面,由不含(C)成分的比较例1的树脂清漆形成的固化膜显示低的密合性。由不含(B)成分的比较例2的树脂清漆形成的固化膜的伸缩性低,伸长率也低。由含有橡胶改性聚酰胺作为弹性体的比较例3的树脂清漆形成的固化膜的伸缩性低,另外光学特性方面也不充分。
产业上的可利用性
由本发明的固化性组合物形成的固化物(伸缩性树脂层)显示出优异的伸缩性及密合性,因此例如可以作为用于保护可穿戴设备的电路基板的密封层来应用或使用。由本发明的固化性组合物形成的伸缩性树脂层在高湿度环境下的长期可靠性方面也可具有优异的性能。
符号说明
1…挠性基板、2…电路部件、3…伸缩性树脂层、100…半导体装置。
Claims (6)
1.一种伸缩性树脂层形成用固化性组合物,含有:
(A)具有聚苯乙烯链的弹性体;
(B)单官能的直链烷基(甲基)丙烯酸酯;
(C)具有脂环基的单官能的(甲基)丙烯酸酯;
(D)具有2个以上的烯属不饱和基的2官能以上的化合物;及
(E)聚合引发剂,
(C)具有脂环基的单官能的(甲基)丙烯酸酯的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量为10质量%~50质量%,
(D)具有2个以上的烯属不饱和基的2官能以上的化合物的含量相对于(A)成分、(B)成分、(C)成分及(D)成分的总量为1质量%~5质量%,
(C)具有脂环基的单官能的(甲基)丙烯酸酯为选自(甲基)丙烯酸3,3,5-三甲基环己酯及(甲基)丙烯酸4-叔丁基环己酯中的一种以上化合物,
由该固化性组合物形成的固化物的伸缩恢复率为80%以上。
2.根据权利要求1所述的伸缩性树脂层形成用固化性组合物,其中,
(A)具有聚苯乙烯链的弹性体是还具有经过氢化的聚二烯链的共聚物。
3.根据权利要求1或2所述的伸缩性树脂层形成用固化性组合物,其中,
(E)聚合引发剂为光自由基聚合引发剂。
4.根据权利要求1或2所述的伸缩性树脂层形成用固化性组合物,其中,
(B)单官能的直链烷基(甲基)丙烯酸酯的直链烷基的碳数为12以下。
5.一种伸缩性树脂层,其为权利要求1~4中任一项所述的伸缩性树脂层形成用固化性组合物的固化物。
6.一种半导体装置,具备权利要求5所述的伸缩性树脂层。
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