CN108410376A - 粘接片 - Google Patents

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Publication number
CN108410376A
CN108410376A CN201810247971.4A CN201810247971A CN108410376A CN 108410376 A CN108410376 A CN 108410376A CN 201810247971 A CN201810247971 A CN 201810247971A CN 108410376 A CN108410376 A CN 108410376A
Authority
CN
China
Prior art keywords
adhesive sheet
adhesive layer
dilatancy
sheet according
adhesive
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201810247971.4A
Other languages
English (en)
Other versions
CN108410376B (zh
Inventor
雷鸣
户高胜则
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Teraoka Seisakusho Co Ltd
Original Assignee
Teraoka Seisakusho Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
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Application filed by Teraoka Seisakusho Co Ltd filed Critical Teraoka Seisakusho Co Ltd
Publication of CN108410376A publication Critical patent/CN108410376A/zh
Application granted granted Critical
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Classifications

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    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B1/00—Layered products having a non-planar shape
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/06—Non-macromolecular additives organic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • C—CHEMISTRY; METALLURGY
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    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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    • C—CHEMISTRY; METALLURGY
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Abstract

本发明公开了一种粘接片，其在基材(1)的一面或两面具有膨胀性粘接剂层(2)，膨胀性粘接剂层(2)含有包含多官能环氧树脂的环氧树脂、作为固化剂的酚醛树脂、作为固化催化剂的咪唑系化合物、以及温敏性发泡剂。该粘接片特别是均衡地具有快速固化性、耐热性、粘接性等特性，且由于充分的填充性，使得热导性等诸特性也优异。

Description

粘接片
本申请是申请日为2016年4月8日、申请号为201680001361.5、发明名称为《粘接片》的中国专利申请的分案申请。
技术领域
本发明涉及一种具有包含环氧树脂、温敏性发泡剂的膨胀性粘接剂层的粘接片。本发明的粘接片用于例如电动发电机中的定子与线圈那样的2个构件之间，在通过加热进行膨胀、发泡、固化并被填充至该间隙中而使构件彼此粘接的用途中有用。
背景技术
环氧树脂粘接剂具有优异的耐热性以及牢固的粘接性，因此被广泛用于构件粘接、结构粘接等。
例如，在近年来迅速普及的电动汽车、混合动力汽车的马达中，缠绕有漆包线的线圈通过环氧树脂被固定于定子铁心。在以前的方法中，通过将绝缘纸插入导体线圈与定子铁心之间，将液状环氧树脂粘接剂注入导体线圈与定子铁心之间的空隙(间隙)中，进行加热使粘接剂固化，从而固定。但是，由于导体线圈与定子铁心的间隙非常窄，粘接剂难以进入，因此会形成空隙，或者在为了避免该状况发生而扩大了间隙的情况下，由于粘接剂的散热性低，因此马达的散热性降低而性能降低，或者为了完全填埋而需要大量的粘接剂。另外，还需要将过量的粘接剂从定子铁心清除的作业。进一步，液状粘接剂通常难以正确控制涂布量、涂布部位。而且，环氧树脂等加热固化性粘接剂通过加热使得粘度降低而容易发生液体流挂，可能会污染被粘物、作业周边，需要使用围栏、障壁等夹具来防止在粘接部以外的液体流挂。由此，液状环氧树脂粘接剂有较多使用时的作业性问题。
于是，提出了使用具有发泡性的环氧树脂粘接剂层的粘接片代替液状环氧树脂粘接剂(专利文献1～4)。然而，在汽车的马达制造中使用的粘接片所要求的特性除作业性以外还涉及许多方面。例如，在粘接剂层的发泡固化工序中，优选使粘接剂保持适当的粘性，且在短时间内均匀地发泡固化。具体而言，要求在180℃发泡固化30分钟左右，优选10分钟左右。另外，发泡固化后的粘接片需要使粘接剂层不脱落这样的柔软性、与基材的密合性。另外，要求不仅在室温，即使在高温气氛下，具体而言在150℃、优选在200℃加热500小时以上，粘接强度也不会降低这样的耐热性，以及即使浸渍在润滑油中粘接强度也不会降低这样的耐油性。另外，必须进行填充，以填埋使导线成束所得的线圈等被粘物的凹凸。为了抑制因马达的温度上升导致的性能降低，也需要散热性以及热导性优异。进一步，为了能够将粘接片高速插入导体线圈与定子之间的窄间隙，要求形状保持性、基材的刚性，需要用于确保定子与被覆导线的绝缘可靠性的绝缘性。从垃圾产生这样的环境考虑出发，也有时要求不使用剥离纸。
专利文献1中是以将粘接片确实地固定于定子的线圈与定子铁心上为目的，关于快速固化性、耐热性(例如抑制高温下的粘接强度降低)并未研究。在专利文献2及3中，由于粘接片的中间层为发泡层，且在其外侧具有不发泡的粘接剂层，因此对凹凸被粘物的填充性、热导性差，另外关于快速固化性、耐热性(例如抑制高温下的粘接强度降低)并未研究。专利文献4中是以粘接性、作业性的提高作为主要目的，关于快速固化性、耐热性(抑制高温下的粘接强度降低)并未研究。
现有技术文献
专利文献
专利文献1：日本特开2011-244596号公报
专利文献2：日本特开2010-261030号公报
专利文献3：日本特开2012-170248号公报
专利文献4：日本特开2013-104044号公报
发明内容
发明要解决的问题
本发明的目的在于提供一种特别是均衡地具有快速固化性、耐热性、粘接性等特性，且由于充分的填充性，使得热导性等诸特性也优异的粘接片。
用于解决问题的方法
本发明是一种具有膨胀性粘接剂层的粘接片，所述膨胀性粘接剂层含有包含多官能环氧树脂的环氧树脂、作为固化剂的酚醛树脂、作为固化催化剂的咪唑系化合物、以及温敏性发泡剂。
发明的效果
本发明的粘接片尽管膨胀性粘接剂层在短时间内发泡固化但仍然具有高柔软性、而且在例如汽车的马达制造中使用的粘接片所要求的各特性也优异。即根据本发明，提供一种特别是均衡地具有快速固化性、耐热性、粘接性等特性均衡、且由于充分的填充性，使得热导性等诸特性也优异的粘接片。
附图说明
图1是表示本发明的粘接片的一个实施方式的示意截面图。
图2是表示本发明的粘接片的一个实施方式的示意截面图。
图3是表示本发明的粘接片的一个实施方式的示意截面图。
图4是表示本发明的粘接片的一个实施方式的示意截面图。
图5是表示本发明的粘接片的一个实施方式的示意截面图。
图6是表示本发明的粘接片的一个实施方式的示意截面图。
图7是表示本发明的粘接片的一个实施方式的示意截面图。
图8是用于说明实施例的剪切粘接力的试验方法的示意图。
图9是用于说明实施例的形状保持性的试验方法的示意图。
具体实施方式
图1～7是表示本发明的粘接片的一个实施方式的示意截面图。在图1所示的实施方式中，在单层基材1的两面设有膨胀性粘接剂层2，膨胀性粘接剂层2包含适量耐热性填料。另外，有时根据需要在一个膨胀性粘接剂层2的表面设有脱模剂层3。
在图2所示的实施方式中，基材1由层叠体构成，该层叠体具有隔着贴合用粘接剂层5使2张树脂膜4层叠而成的结构。贴合用粘接剂层5包含适量耐热性填料。然后，在基材1的两面设有膨胀性粘接剂层2，膨胀性粘接剂层2包含适量耐热性填料。另外，有时根据需要在一个膨胀性粘接剂层2的表面设有脱模剂层3。
在图3所示的实施方式中，基材1由层叠体构成，该层叠体具有隔着贴合用粘接剂层5使树脂膜4与无纺布6层叠而成的结构。在无纺布6中含浸有包含适量耐热性填料的树脂组合物。其它构成与图2同样。
在图4所示的实施方式中，基材1由层叠体构成，该层叠体具有隔着贴合用粘接剂层5使树脂膜4与纸6层叠而成的结构。其它构成与图2同样。
在图5所示的实施方式中，基材1由层叠体构成，该层叠体在树脂膜4的两面具有功能性粘接剂层8。功能性粘接剂层8包含适量耐热性填料以及纤维状填料。其它构成与图2同样。
在图6所示的实施方式中，在单层基材1的一面设有膨胀性粘接剂层2，膨胀性粘接剂层2包含适量耐热性填料。另外，在膨胀性粘接剂层2或基材1的表面设有脱模剂层3。
在图7所示的实施方式中，没有基材1，在膨胀性粘接剂层2的两面设有剥离膜9。膨胀性粘接剂层2包含适量耐热性填料。这样的无基体型的粘接片剥下剥离膜9而使用。
下面，对本发明的粘接片的各构成进行说明。
[基材1]
本发明中的基材1如图1～6所示是用于支撑膨胀性粘接剂层2的构件。但也可以如图7所示是没有基材1的无基体型的粘接片。
基材1优选具有耐热性。耐热性的水平根据使用的用途而不同，例如基材1的熔融温度优选为200℃以上，更优选为250℃以上。另外例如依照UL-746B测定的基材1的连续使用温度优选为100℃以上，更优选为150℃以上。另外，在基材1包含树脂的情况下，该树脂的玻璃化转变点优选为80℃以上，更优选为140℃以上，特别优选为200℃以上。
基材1可以如图1以及6所示为由一个构件构成的单层基材，也可以如图2～4所示为由具有通过贴合用粘接剂使一个构件与其它构件贴合的层叠结构的层叠体构成的基材，还可以如图5所示为由在构件的一面或两面具有功能性粘接剂层的层叠体构成的基材。基材1可以具有柔软性，或也可以具有回弹性，其性状根据用途适当选择。在要求粘接片的强度(刚度)、形状保持性的用途中，基材1优选如图2～4所示为由具有通过贴合用粘接剂使一个构件与其它构件贴合的层叠结构的层叠体构成的基材、以及如图5所示为由在构件的一面或两面具有功能性粘接剂层的层叠体构成的基材，该构件更优选为选自由树脂膜4、无纺布6以及纸7组成的组中的一种以上构件。进一步具体而言，更优选为如图2～4所示由具有通过贴合用粘接剂使树脂膜4与无纺布6、或树脂膜4与纸7、或树脂膜4与树脂膜4贴合的层叠结构的层叠体构成的基材1。这些优选的实施方式在例如马达槽的制造等用途中非常适宜。这是因为，在这样的用途中，需要将粘接片高速且稳定地插入槽那样的窄间隙，因此要求强度(刚度)高且弯曲后的形状保持性优异的基材。
作为树脂膜4的具体例子，可列举聚对苯二甲酸乙二酯(PET)、聚对苯二甲酸丁二酯、聚萘二甲酸乙二酯(PEN)、芳香族聚酯等聚酯系树脂；聚碳酸酯；聚芳酯；聚氨酯；聚酰胺、聚醚酰胺等聚酰胺系树脂；聚酰亚胺、聚醚酰亚胺、聚酰胺酰亚胺等聚酰亚胺系树脂；聚砜、聚醚砜等聚砜系树脂；聚醚酮、聚醚醚酮等聚醚酮系树脂；聚苯硫醚(PPS)；改性聚苯醚。也可以并用2种以上的树脂膜4。其中，从耐热性、绝缘性以及成本的平衡的观点考虑，优选聚萘二甲酸乙二酯(PEN)。
作为无纺布6的具体例子，可列举包含纤维素纤维、聚酯纤维、尼龙纤维、芳族聚酰胺纤维、聚苯硫醚纤维、液晶聚合物纤维、玻璃纤维、金属纤维、碳纤维等纤维的无纺布。也可以并用2种以上的无纺布6。其中，优选芳族聚酰胺纤维无纺布、玻璃纤维无纺布、聚苯硫醚纤维无纺布、耐热尼龙纤维无纺布、耐热聚酯纤维无纺布。从耐热性、热导性以及防止膨胀性粘接剂层2侵入等的观点考虑，优选在无纺布6中含浸包含耐热性填料的树脂组合物。作为树脂的具体例子，可列举聚酯树脂、聚酰胺树脂、丁缩醛树脂、聚氨酯树脂、丙烯酸树脂、环氧树脂。其中，优选聚氨酯树脂。耐热性填料的具体例子与后述的各粘接剂所含的耐热性填料的具体例子相同。
作为纸7，优选吸水性低、耐热性高的纸。特别优选由全芳香族聚酰胺聚合物构成的高耐热性纸。纸7也可以为包含2种以上纤维的混合纸的形态。
贴合用粘接剂层5以及功能性粘接剂层8全都为使用粘接剂形成的层。而且贴合用粘接剂层5是以贴合构成基材的构件为目的而设置的层，但也可以根据需要适量填充赋予热导性、绝缘性、耐热性等特殊功能的添加剂。功能性粘接剂层8是以通过包含除粘接剂以外的成分(填料等)，从而对粘接片赋予某些功能(耐热性、热导性、强度(刚度)等)为目的而设置的层。功能性粘接剂层8例如设置在选自由树脂膜4、无纺布6以及纸7组成的组中的构件的一面或两面。
构成贴合用粘接剂层5以及功能性粘接剂层8的粘接剂没有特别限制。也可以适宜使用与后述的构成膨胀性粘接剂层2的粘接剂相同的粘接剂。特别是从对膜4等的润湿性、粘接均匀性的观点考虑，优选包含软化点低的成分、液状成分。另外，从层叠基材的平滑性的观点考虑，优选固化收缩率小的环氧树脂。构成贴合用粘接剂层5以及功能性粘接剂层8的粘接剂也可以含有温敏性发泡剂，也有时优选不含有温敏性发泡剂，不进行发泡。
从耐热性、热导性的观点考虑，构成贴合用粘接剂层5以及功能性粘接剂层8的粘接剂优选包含耐热性填料。耐热性填料的种类没有特别限制，例如可列举氧化铝、氧化镁、氧化钙、氢氧化铝、氢氧化镁、氮化硼、氮化硅、氧化硅、滑石(硅酸镁)等无机填料。也可以并用2种以上的耐热性填料。耐热性填料的含量相对于粘接剂中的树脂成分100质量份优选为10～300质量份，更优选为50～150质量份。
构成贴合用粘接剂层5以及功能性粘接剂层8的粘接剂也可以包含纤维状填料作为耐热性填料。特别是构成功能性粘接剂层8的粘接剂优选包含纤维状填料。纤维状填料在提高粘接片的强度(刚度)方面有用，作为纤维状填料的具体例子，可列举聚酯纤维、聚酰胺纤维、玻璃纤维。也可以并用2种以上的纤维状填料。其中，优选玻璃纤维。纤维状填料的平均纤维直径优选为1～20μm，平均纤维长度优选为10～150μm。
为了提高与膨胀性粘接层2的密合性，也可以对基材1实施电晕处理、底漆处理等。
基材1的厚度只要根据使用用途适当选择即可，通常为2～200μm。特别是在用于马达的定子与线圈的粘接绝缘等的情况下，优选为9～100μm，更优选为12～50μm。
[膨胀性粘接剂层2]
本发明的膨胀性粘接剂层2含有包含多官能环氧树脂的环氧树脂、作为固化剂的酚醛树脂、作为固化催化剂的咪唑系化合物、以及温敏性发泡剂。
膨胀性粘接剂层2优选包含环氧树脂作为主要成分。多官能环氧树脂的种类没有限制，优选苯酚酚醛清漆型、甲酚酚醛清漆型等酚醛清漆型环氧树脂以及它们的混合物。如果使用酚醛清漆型环氧树脂，则由于固化物的玻璃化转变点变高，因此即使高温下也有粘接力稳定的倾向。
作为环氧树脂，也可以并用除多官能环氧树脂以外的环氧树脂。通过混合使用多官能环氧树脂以及除其以外的环氧树脂，从而能够容易且详细调整环氧树脂的软化点、熔融粘度、玻璃化转变点、储能模量等物性。通常，如果混合软化点低或液状的环氧树脂，则能够提高粘接剂层加热时的流动性以及固化前后的可挠性。另一方面，如果混合软化点高或半固体或固体的环氧树脂，则能够降低粘接剂层表面的粘着性。另外，为了使温敏性发泡剂所含的粉状或粒状的热膨胀性微胶囊等成分预分散、为了均匀混合环氧树脂成分，也可以使用液状的环氧树脂。
作为这样的能够混合的环氧树脂的具体例子，可列举双酚A型、二聚酸改性双酚A型、双酚F型等双酚型环氧树脂；己二醇二缩水甘油醚等具有脂肪族骨架的环氧树脂；苯氧树脂(由双酚类与环氧氯丙烷合成的聚羟基聚醚)；结晶环氧树脂。结晶环氧树脂在常温下为无粘着性的固体，而在熔点以上熔融粘度大大降低，因此在熔点以上作为反应性稀释剂起作用。因此，如果粘接层包含结晶环氧树脂，则能够进一步提高粘接层加热时的流动性，对粘接层的热膨胀起有利作用。另外，由于在室温下为非粘着性的固体，因此有助于降低粘接层表面的粘着性或使粘接层表面为非粘着性。在通过熔融涂布法形成粘接层的情况下，通过加热至结晶环氧树脂的熔点以上，能够降低环氧树脂的熔融粘度，提高熔融涂布的速度。
环氧树脂的数均分子量以通过GPC的标准聚苯乙烯换算计，通常为100～60000。环氧树脂的环氧当量通常为50～30000g/eq。
作为在膨胀性粘接剂层2中使用的环氧树脂的固化剂，使用酚醛树脂。在本发明中，将酚醛树脂用作固化剂，与后述的作为固化催化剂的咪唑系化合物组合使用，在缩短固化时间且提高耐热性方面很重要。另外，通过使用酚醛树脂作为固化剂，从而使耐热性、电特性等的设计变得容易。酚醛树脂的添加量理论上以使酚醛树脂的羟基当量数相对于环氧树脂的环氧当量数为1比1附近的方式决定。酚醛树脂的羟基当量数相对于环氧树脂的环氧当量数的比率通常为0.5～2.0，优选为0.8～1.2。
作为在膨胀性粘接剂层2中使用的环氧树脂的固化催化剂，使用咪唑系化合物。在本发明中，将咪唑系化合物用作固化催化剂，与作为固化剂的酚醛树脂组合使用，在缩短固化时间且提高耐热性方面很重要。例如，在以前技术中，有时不使用酚醛树脂作为固化剂，而是大量使用咪唑系化合物作为固化剂，在这种情况下，难以得到本发明那样优异的长期耐热这样的耐久性。在本发明中，咪唑系化合物用作固化催化剂，即仅以作为催化剂的量(少量)使用，且将酚醛树脂用作固化剂，即以作为固化剂的量(大量)使用，由此得到本发明的效果。另外，咪唑系化合物与其它固化催化剂相比，能够单独作为催化剂使用且还具有粒径非常细的粒度，因此有容易使用这样的优点。
作为咪唑系化合物的具体例子，可列举2-苯基-4,5-二羟基甲基咪唑、2-苯基-4-甲基咪唑、2-乙基-4-甲基咪唑、2,4-二乙基咪唑、2-苯基-4-甲基-5-羟基咪唑等咪唑衍生物。也可以并用2种以上的咪唑系化合物。其中，优选2-苯基-4,5-二羟基甲基咪唑。咪唑系化合物的含量相对于膨胀性粘接剂层中的树脂成分100质量份优选为0.1～1.0质量份，更优选为0.3～0.8质量份。
作为在膨胀性粘接剂层2中使用的温敏性发泡剂，例如可列举碳酸铵、碳酸氢铵、亚硝酸铵、硼氢化铵、叠氮化物类等无机系发泡剂；三氯一氟甲烷等氟代烷烃、偶氮二异丁腈等偶氮系化合物、对甲苯磺酰肼等肼系化合物、对甲苯磺酰氨基脲等氨基脲系化合物、5-吗啉基-1,2,3,4-噻三唑等三唑系化合物、N,N-二亚硝基对苯二甲酰胺等N-亚硝基化合物等有机系发泡剂；使由烃系化合物等构成的热膨胀剂微胶囊化而成的热膨胀性微胶囊。也可以并用2种以上的温敏性发泡剂。其中，从不妨碍环氧树脂的固化、减少对环氧树脂物性造成的不良影响的观点考虑，优选热膨胀性微胶囊。
热膨胀性微胶囊为以具有阻气性的热塑性树脂为壳，在壳的内部内含热膨胀剂的微胶囊。对热膨胀性微胶囊进行加热时，壳的热塑性树脂软化，热膨胀剂的体积增大，从而使胶囊膨胀。例如，能够将低沸点的烃系化合物的气化用于胶囊的膨胀。
热膨胀性微胶囊的膨胀(发泡)温度优选为环氧树脂的软化点以上，且环氧树脂的固化反应的活化温度以下。如果该发泡温度为环氧树脂的软化点以上，则在变软的环氧树脂中能够使热膨胀剂充分膨胀，能够使发泡后的膨胀性粘接剂层2的厚度变得均匀。另外，如果该发泡温度为环氧树脂的固化反应的活化温度以下，则能够防止环氧树脂在发泡前固化。进一步，通过将环氧树脂的软化点设为固化反应的活化温度以下，从而在粘接片的制造工序包含熔融或溶液涂布的情况下，能够防止环氧树脂在这些涂布工序以及伴随其的干燥工序中发生凝胶化。
环氧树脂的软化点可以使用JIS K 2207规定的环球式软化点试验法进行测定。热膨胀性微胶囊的发泡温度是指热膨胀性微胶囊发生体积变化的温度，例如可以选自70℃以上200℃以下，优选100℃以上180℃以下的范围。
温敏性发泡剂的含量以及体积膨胀率可以根据固化的膨胀性粘接剂层2所要求的强度和粘接力、粘接片所要求的膨胀率等适当决定。温敏性发泡剂的含量相对于膨胀性粘接剂层2中的树脂成分100质量份优选为0.5～20质量份，更优选为2～15质量份。发泡后的粘接片的厚度的增加倍数例如可以设为1.1倍以上10倍以下。
从与基材1的密合性、弯曲粘接片时的柔软性、粘接剂涂布时的流平性、防止加热发泡固化时的液体流挂等的观点考虑，膨胀性粘接剂层2中优选添加其它树脂(耐热性树脂等)。作为其它树脂的具体例子，可列举聚酯树脂、丁缩醛树脂、聚氨酯树脂、羧基末端丁腈橡胶(CTBN)、环氧改性丁二烯。其中，从柔软性、粘接性的观点考虑，尤其优选为聚氨酯树脂。
聚氨酯树脂通常为包含由多元醇单体单元构成的软段、以及由多官能异氰酸酯化合物或低分子二醇单体单元构成的硬段的树脂。在聚氨酯树脂中使用的多元醇为具有2个以上羟基的化合物。从提高橡胶弹性伸长恢复率等特性的观点考虑，多元醇的羟基数优选为2～3，更优选为2。作为多元醇，例如可以使用聚酯多元醇、聚醚多元醇、聚己内酯多元醇、聚碳酸酯多元醇、蓖麻油系多元醇。也可以并用2种以上的多元醇。
作为用作用于将多元醇交联的交联剂的多官能异氰酸酯化合物，可以使用例如多官能脂肪族系异氰酸酯化合物、多官能脂环族系异氰酸酯化合物、多官能芳香族系异氰酸酯化合物。另外，也可以使用这些化合物的三羟甲基丙烷加合物、与水反应而得的缩二脲物、具有异氰脲酸酯环的3聚体。也可以并用2种以上的多官能异氰酸酯化合物。
作为多官能脂肪族系异氰酸酯化合物的具体例子，可列举三亚甲基二异氰酸酯、四亚甲基二异氰酸酯、六亚甲基二异氰酸酯、五亚甲基二异氰酸酯、1,2-亚丙基二异氰酸酯、1,3-亚丁基二异氰酸酯、十二亚甲基二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯。
作为多官能脂环族系异氰酸酯化合物的具体例子，可列举1,3-环戊烯二异氰酸酯、1,3-环己烷二异氰酸酯、1,4-环己烷二异氰酸酯、异佛尔酮二异氰酸酯、氢化二苯基甲烷二异氰酸酯、氢化亚二甲苯基二异氰酸酯、氢化甲苯二异氰酸酯、氢化四甲基亚二甲苯基二异氰酸酯。
作为多官能芳香族系二异氰酸酯化合物的具体例子，可列举亚苯基二异氰酸酯、2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、2,2'-二苯基甲烷二异氰酸酯、4,4'-二苯基甲烷二异氰酸酯、4,4'-甲苯胺二异氰酸酯、4,4'-二苯基醚二异氰酸酯、4,4'-二苯基二异氰酸酯、1,5-萘二异氰酸酯、亚二甲苯基二异氰酸酯。
聚氨酯树脂通过使含有以上说明的多元醇与多官能异氰酸酯化合物的组合物固化而得到。特别是从橡胶弹性伸长恢复率等特性的观点考虑，优选低结晶性的线性聚酯系聚氨酯树脂，更优选己二醇共聚酯系聚氨酯树脂，聚四亚甲基二醇系聚氨酯树脂。
聚氨酯树脂的含量在膨胀性粘接剂层2中的树脂成分100质量份中优选为60质量份以下。
从耐热性、热导性的观点考虑，膨胀性粘接剂层2优选包含耐热性填料。耐热性填料的种类没有特别限制，例如可列举氧化铝、氧化镁、氧化钙、氢氧化铝、氢氧化镁、氮化硼、氮化硅、氧化硅、滑石(硅酸镁)等无机填料。也可以并用2种以上的耐热性填料。耐热性填料的含量相对于粘接剂中的树脂成分100质量份，优选为20～300质量份，更优选为50～100质量份。
膨胀性粘接剂层2也可以根据需要包含酚系抗氧化剂、硫系抗氧化剂等抗氧化剂、环氧改性烷氧基硅烷等硅烷偶联剂、气相二氧化硅等触变剂、用于辨别的颜料、染料等添加剂。
膨胀性粘接剂层2可以为连续层，也可以为由多个条纹、点等图案构成的不连续层。进一步，也可以在膨胀性粘接剂层2的表面形成压花等凹凸。通过将膨胀性粘接剂层2设为不连续的层、或在粘接剂层的表面形成压花等凹凸，能够降低膨胀性粘接剂层2表面的粘着性或使粘接剂层实质上为非粘着性，或能够调整粘接力，或能够仅在必要的部分形成粘接剂层。另外，这样的膨胀性粘接剂层2表面的不均匀性在发泡时减轻或消除，因此也难以因其不均匀性而对粘接力造成不良影响。
[脱模剂层3]
就一般的两面粘接片而言，通常为了防止粘接剂层的粘连而设置剥离纸。然而近年来，从环境考虑出发，也有时要求不使用剥离纸的粘接片。另外，一般而言，多数情况期望粘接剂层具有能够临时固定于被粘物的程度的粘着性，但也有时有利的是加热前粘接剂层为非粘着性(无粘性)。例如，如果热膨胀性粘接剂层2为非粘着性，则进一步提高粘接片的操作性以及作业性。具体而言，在将定子铁心与线圈粘接的情况下，具有非粘着性的粘接剂层的粘接片能够更加顺畅地插入定子铁心的间隙，在插入粘接片而变得更窄的空隙能够更加顺畅地插入线圈。从这样的观点考虑，在本发明的粘接片中，优选在至少一个膨胀性粘接剂层2的表面涂布脱模剂。进一步，在基材1的两面具有膨胀性粘接剂层2的情况下，优选在至少一个膨胀性粘接剂层2的表面涂布脱模剂。
在以前技术中，脱模剂通常涂布在无粘接剂层的基材的表面。另一方面，在本发明中，以创新的构思实现了将脱模剂直接涂布在膨胀性粘接剂层2的表面，且对粘接性等特性无影响。为了减少对膨胀性粘接剂层2的不良影响，本发明中使用的脱模剂必须满足以下要件(a)和(b)中任一个。
(a)构成脱模剂的成分为低分子量，在低温下(使用前保管粘接片时的温度)发挥脱模功能，但在高温(使用时粘接片的发泡固化温度)下其成分分解、蒸发或升华而几乎丧失脱模功能。
(b)脱模剂的涂布量少，在使用时通过粘接片中的膨胀性粘接剂层2的软化、熔融、流动以及发泡进行的从搅拌到固化的过程中，脱模剂进入粘接剂层中而几乎丧失脱模功能。
作为脱模剂的具体例子，可列举石蜡、长链烷基系化合物等有机系热熔融聚合物；有机硅、碳酸钙、氧化硅微粒等无机系微粒。其中，从粘接片的保存稳定性、粘接性的观点考虑，优选长链烷基系化合物。有机或无机系油由于污染粘接片的生产线、使用线而且大幅度降低膨胀性粘接剂层2的粘接性，因此不优选。
作为长链烷基系化合物，可以使用市售的长链烷基系脱模剂。例如有作为有机溶剂可溶型长链烷基系脱模剂的“PEELOIL(注册商标)1010”(Lion Specialty Chemicals公司制)、作为水分散型长链烷基系脱模剂的“NC003”(中京油脂公司制)。特别是从防止有机溶剂侵入粘接剂层中、粘接剂成分渗出的观点考虑，优选水分散型长链烷基系化合物。
水分散型长链烷基系化合物只要使用水稀释为适当的浓度，以干燥后脱模剂层3的厚度为0.02～0.2μm的方式进行涂布即可。如果其厚度为0.02μm以上，则有脱模性稳定的倾向，如果为0.2μm以下则有膨胀性粘接剂层2发泡固化时的粘接性难以降低的倾向。为了将水分散型长链烷基系化合物薄膜涂布在环氧树脂粘接剂层那样的极性较低层的表面上，优选使用适当的润湿性提高剂。作为润湿性提高剂的具体例子，可列举乙炔二醇。
[粘接片]
本发明的粘接片为具有以上说明的膨胀性粘接剂层2的粘接片，更具体而言，其为在基材1的一面或两面具有膨胀性粘接剂层2的粘接片、或无基材1的无基体型的粘接片。粘接片也可以具有除基材1以及膨胀性粘接剂层2以外的层或构件，例如脱模剂层3、脱模膜9。
本发明的粘接片发泡固化前的厚度例如为10～1000μm。在将本发明的粘接片插入例如定子铁心与线圈之间那样窄的间隙的情况下，发泡固化前的厚度优选为250μm以下，更优选为20～200μm。
本发明的粘接片的初期粘接性优异而且耐热性也优异。具体而言，膨胀性粘接剂层2发泡固化后的粘接片依照JIS Z 1541的剪切粘接力在室温(23℃)时优选为200N/cm2以上，更优选为300N/cm2以上，在200℃加热时优选为50N/cm2以上，更优选为100N/cm2以上。
本发明的粘接片的弯曲强度与弯曲后的形状保持性优异。具体而言，膨胀性粘接剂层2发泡固化前的粘接片依照JIS P 8125的弯矩优选为40～600gf·cm，更优选为50～150gf·cm。而且，膨胀性粘接剂层发泡固化前的粘接片通过以下方法测定的形状保持率优选为70％以上，更优选为90％以上。
(形状保持率)
在L字型铝框上放置膨胀性粘接剂层发泡固化前的粘接片，将按压夹具从粘接片的上面以45度的角度朝着角部进行按压，以成为L字型的方式实施弯曲加工，取出试验片，5秒后测定试验片的角度，通过下式进行计算。
形状保持率(％)＝90度÷(弯曲加工5秒后的角度)×100(％)
本发明的粘接片的制造方法没有特别限制。两面粘接片可以通过在基材1的一个表面上形成第1膨胀性粘接剂层2，接着在基材1的另一个表面上形成第2膨胀性粘接剂层2而制造。无基体型的粘接片可以通过在剥离膜9的表面上形成膨胀性粘接剂层2，接着在膨胀性粘接剂层2上贴合另一个剥离膜9而制造。但也可以是除它们以外的方法，例如也可以同时涂布膨胀性粘接剂，不使用单面剥离膜9进行制作。
膨胀性粘接剂层2例如可以通过溶液涂布法、熔融涂布法、熔融挤出法、轧制法等以前已知的方法形成。熔融涂布法可以以无溶剂进行，不需要溶剂的除去工序、处理设备等，因此从生产率以及经济性方面出发优选。在使用熔融涂布法的情况下，优选环氧树脂包含结晶环氧树脂。在这种情况下，通过加热至结晶环氧树脂的熔点以上，能够降低环氧树脂的熔融粘度，能够提高熔融涂布的速度。
实施例
下面，通过实施例进一步说明本发明，但本发明不限于这些实施例。
＜基材制作用粘接剂的调制＞
以表1所示的量(质量份)混合以下各成分，得到基材制作用粘接剂(配合1～5)。
“EP1”：环氧树脂(液状、粘度13,500mPa·s(25℃)、环氧当量189g/eq、BPA型、标准液状品)
“EP2”：环氧树脂(半固体、环氧当量173g/eq、多官能苯酚酚醛清漆型、耐热性型)
“EP3”：环氧树脂(软化点70℃、环氧当量210g/eq、特殊酚醛清漆型、耐热性型)
“EP4”：环氧树脂(软化点92℃、环氧当量200g/eq、特殊多官能型、高耐热性型)
“EP5”：环氧树脂(软化点86℃、环氧当量230g/eq、萘环型、耐热性·韧性型)
“EP6”：环氧树脂(软化点92℃、环氧当量395g/eq、异氰酸酯改性型、高Tg·高韧性·强粘接型)
“PU”：线性聚酯聚氨酯树脂(软化点87℃、分子量222300、羟基含量0.1％、粘接性·柔软性型)
“H”：热膨胀性微胶囊(平均粒径9μm、膨胀起始温度120～130℃、最大膨胀温度145～155℃)
“T1”：酚醛树脂(软化点87℃、羟基当量178g/eq、酚醛清漆型、高耐热性型)
“T2”：异氰酸酯系固化剂(日本聚氨酯公司制、CORONATE(注册商标)L)
“T3”：2-苯基-4,5-二羟基甲基咪唑(四国化成工业公司制、商品名2PHZ-PW、熔点220℃、活性区域141～153℃、起始区域153～168℃)
“J1”：氧化镁(平均粒径3μm)
“J2”：硅酸镁(平均粒径5μm)
“J3”：玻璃纤维(平均纤维直径6μm、平均纤维长度50μm)
“MEK”：甲基乙基酮
[表1]
表1(基材制作用粘接剂)
＜基材的制作＞
作为基材用构件，准备以下各构件F1～F6、P。
“F1”：聚萘二甲酸乙二酯(PEN)膜(帝人杜邦膜公司制、TEONEX(注册商标)Q51、厚度38μm)
“F2”：聚萘二甲酸乙二酯(PEN)膜(帝人杜邦膜公司制、TEONEX(注册商标)Q51、厚度12μm)
“F3”：聚苯硫醚(PPS)膜(东丽公司制、TORELINA(注册商标)#50-2030、厚度50μm)
“F4”：聚对苯二甲酸乙二酯(PET)膜(东丽公司制、LUMIRROR(注册商标)S-10、厚度50μm)
“F5”：聚对苯二甲酸乙二酯(PET)膜(东丽公司制、LUMIRROR(注册商标)S-10、厚度38μm)
“F6”：含浸有粘接剂(配合5)的芳族聚酰胺与聚酯的混合无纺布(该无纺布F6如下得到：将作为聚氨酯树脂组合物的粘接剂(配合5)以干燥后的涂布质量为约40g/m2的方式含浸在芳族聚酰胺与聚酯的混合无纺布(帝人公司制、CONEX(注册商标)、厚度40μm(20g/m2))，之后干燥而得到。)
“P”：芳香族聚酰胺纸(杜邦公司制、NOMEX(注册商标)、厚度60μm)
使用以上各构件F1～F6、P以及基材制作用粘接剂(配合1～5)，制作以下基材K1a～K10。
“K1a”：使用粘接剂(配合1)将2张PEN膜F1贴合而得的层叠基材。(该层叠基材K1a如下得到：在PEN膜F1的一面以干燥后的厚度为30μm的方式涂布粘接剂(配合1)，之后干燥，使用加热至100℃的热辊将另一个PEN膜F1压制并贴合而得到。)
“K1b”：使用粘接剂(配合2)将2张PEN膜F1贴合而得的层叠基材。(该层叠基材K1b除了使用粘接剂(配合2)以外与层叠基材K1a同样地操作得到。)
“K2”：使用粘接剂(配合1)将PEN膜F1与PET膜F5贴合而得的层叠基材。(该层叠基材K2除了使用PEN膜F1以及PET膜F5以外与层叠基材K1a同样地操作得到。)
“K3”：使用粘接剂(配合1)将2张PET膜F5贴合而得的层叠基材。(该层叠基材K3除了使用2张PET膜F5以外与层叠基材K1a同样地操作得到。)
“K4”：使用粘接剂(配合1)将PEN膜F1与芳香族聚酰胺纸P贴合而得的层叠基材。(该层叠基材K4除了使用PEN膜F1以及芳香族聚酰胺纸P以外与层叠基材K1a同样地操作得到。)
“K5a”：使用粘接剂(配合2)将PEN膜F1与含浸有粘接剂(配合5)的无纺布F6贴合而得的层叠基材。(该层叠基材K5a如下得到：在PEN膜F1的一面以干燥后的厚度为25μm的方式涂布粘接剂(配合2)，之后干燥，使用加热至100℃的热辊将含浸有粘接剂(配合5)的无纺布F6压制并贴合而得到。)
“K5b”：使用粘接剂(配合3)将PEN膜F1与含浸有粘接剂(配合5)的无纺布F6贴合而得的层叠基材。(该层叠基材K5b除了使用粘接剂(配合3)以外与层叠基材K5a同样地操作得到。)
“K6”：在1张PEN膜F1的两面具有由粘接剂(配合4)构成的层的基材。(该基材K6如下得到：分别对PEN膜F1的两面以干燥后的厚度为15μm的方式涂布粘接剂(配合4)，之后进行干燥而得到。)
“K7”：使用粘接剂(配合4)将2张PEN膜F2贴合而得的层叠基材。(该基材K7如下得到：在PEN膜F2的一面以干燥后的厚度为30μm的方式涂布粘接剂(配合4)，之后进行干燥，使用加热至100℃的热辊将另一个PEN膜压制并贴合而得到。)
“K8”：直接使用1张PEN膜F1的基材。
“K9”：直接使用1张PPS膜F3的基材。
“K10”：直接使用1张PET膜F4的基材。
＜膨胀性粘接剂层用粘接剂的调制＞
以表2所示的量(质量份)混合以下各成分，得到膨胀性粘接剂(配合2～3以及6～8)。另外，配合2～3的粘接剂为与作为基材制作用粘接剂而预先调制的配合2～3相同组成的物质。
“EP1”：环氧树脂(液状、粘度13,500mPa·s(25℃)、环氧当量189g/eq、BPA型、标准液状品)
“EP2”：环氧树脂(半固体、环氧当量173g/eq、多官能苯酚酚醛清漆型、耐热性型)
“EP3”：环氧树脂(软化点70℃、环氧当量210g/eq、特殊酚醛清漆型、耐热性型)
“EP4”：环氧树脂(软化点92℃、环氧当量200g/eq、特殊多官能型、高耐热性型)
“EP5”：环氧树脂(软化点86℃、环氧当量230g/eq、萘环型、耐热性·韧性型)
“EP6”：环氧树脂(软化点92℃、环氧当量395g/eq、异氰酸酯改性型、高Tg·高韧性·强粘接型)
“EP7”：环氧树脂(软化点92℃、环氧当量218g/eq、邻甲酚酚醛清漆型、粘接性型)
“EP8”：环氧树脂(软化点70℃、环氧当量288g/eq、酚醛清漆型、高韧性型)
“PU”：线性聚酯聚氨酯树脂(软化点87℃、分子量222300、羟基含量0.1％、粘接性·柔软性型)
“H”：热膨胀性微胶囊(平均粒径9μm、膨胀起始温度120～130℃、最大膨胀温度145～155℃)
“T1”：酚醛树脂(软化点87℃、羟基当量178g/eq、酚醛清漆型、高耐热性型)
“T2”：异氰酸酯系固化剂(日本聚氨酯公司制、CORONATE(注册商标)L)
“T3”：2-苯基-4,5-二羟基甲基咪唑(四国化成工业公司制、商品名2PHZ-PW、熔点220℃、活性区域141～153℃、起始区域153～168℃)
“J1”：氧化镁(平均粒径3μm)
“J2”：硅酸镁(平均粒径5μm)
“J3”：玻璃纤维(平均纤维直径6μm、平均纤维长度50μm)
“MEK”：甲基乙基酮
[表2]
表2(膨胀性粘接剂层用粘接剂)
＜脱模剂X的调制＞
混合水分散型长链烷基系化合物(中京油脂公司制、商品名NC003)10质量份、乙炔二醇(空气化工产品公司制)0.4质量份、蒸馏水389.6质量份，从而得到脱模剂X。
＜实施例1～10、参考例1～3以及比较例1～2＞
在基材K1a～K10的一面以干燥后的厚度为约35μm(实施例8中约25μm、实施例9以及10中约30μm)的方式涂布膨胀性粘接剂(配合2～3以及6～7)，之后通过于90℃干燥5分钟而将溶剂除去，形成膨胀性粘接剂层。用加热至100℃的热辊在该膨胀性粘接剂层的表面压制一面经有机硅脱模处理的厚度38μm的聚酯膜，得到第1工序品。在该第1工序品的基材的另一面以干燥后的厚度为约35μm(实施例8中约25μm、实施例9以及10中约30μm)的方式涂布相同种类的膨胀性粘接剂组合物，之后通过于90℃干燥5分钟而将溶剂除去，形成膨胀性粘接剂层。使用加热至100℃的热辊在该膨胀性粘接剂层的表面将一面经有机硅脱模处理的厚度38μm的聚酯膜压制，得到第2工序品。接着，剥离一个聚酯膜，在该剥离面上涂布约10g/m2脱模剂X，之后于90℃干燥3分钟，在膨胀性粘接剂层上形成脱模剂层。接着，将另一个聚酯膜一边剥离一边卷绕，得到实施例1～10、参考例1～3以及比较例1～2的粘接片。
＜实施例11＞
在一面有机硅重剥离·脱模处理聚酯膜38μm上以干燥后的厚度为25μm的方式涂布膨胀性粘接剂(配合8)，之后通过于90℃干燥5分钟而将溶剂除去，形成膨胀性粘接剂层。在该膨胀性粘接剂层的表面贴合一面有机硅轻剥离·脱模处理聚酯膜38μm并卷绕，从而得到实施例11的粘接片。该粘接片使用时剥离两面的脱模处理聚酯膜，作为仅由膨胀性粘接剂层构成的无基体型的粘接片使用。
对于以上的实施例1～11、参考例1～3以及比较例1～2的粘接片，按照以下的方法进行评价。将结果示于表3～5中。
[粘接片的厚度]
发泡前的粘接片的厚度依据JIS Z 0237“粘着胶带·粘着片试验方法”，通过使用测厚规的试验方法进行测定。发泡后的粘接片的厚度如下测定：将发泡前的粘接片切出50×50mm的尺寸，纵向悬挂在热风干燥机上，在170℃、10分钟的条件下进行发泡固化，于室温冷却2小时，之后通过与上述相同的方法测定。
[拉伸强度]
依照JIS C 2107“电绝缘用粘着胶带试验方法”，测定发泡后的粘接片的拉伸强度(N/10mm)。另外，粘接片的发泡方法与上述粘接片的厚度项目所记载的方法相同(以下同样)。
[伸长率]
依照JIS C 2107“电绝缘用粘着胶带试验方法”，测定发泡后的粘接片的伸长率(％)。
[绝缘击穿电压]
依照JIS C 2107“电绝缘用粘着胶带试验方法”，测定发泡后的粘接片的绝缘击穿电压(kV)。
[剪切粘接力(室温(23℃)、200℃加热)]
依照JIS Z 1541“超强力双面粘着胶带”所记载的拉伸剪切粘接力试验方法，测定以下所示的发泡后的粘接片的剪切粘接力。作为被粘物，使用SPCC板(日新制钢公司制、商品名SPCC-SB NCB、1.0mm厚、12×100mm)。试样粘贴面积设为10×10mm，发泡固化条件设为170℃、10分钟，拉伸速度设为200mm/分钟。首先如图8(A)所示，在SPCC板11上放置发泡前的粘接片10，进一步隔着2个金属塞尺12放置另一个SPCC板11，接着如图8(B)所示，使粘接片10发泡固化，对该发泡后的粘接片10进行拉伸剪切粘接力测定(室温(23℃)、200℃加热)。
[热导率]
使用京都电子工业公司制的快速热导率计，以薄膜测定模式测定发泡后的粘接片的热导率。具体而言，在铝板(厚度10mm、250×350mm)上放置热导率已知的3种参考物(reference block)，在其上放置测定用试验片(45×100mm)，进一步在其上放置装备有加热线和热电偶的热导率测定用的传感器探头(商品名PD-11、40×97mm、820g)，开始测定。作为参考物，使用发泡聚乙烯(热导率0.0347W/mK)、有机硅橡胶(热导率0.236W/mK)、石英玻璃(热导率1.416)。
[强度(刚度)]
作为发泡前的粘接片的强度(刚度)，测定弯曲发泡粘接片时的抵抗力。具体而言，依照JIS P 8125“纸以及纸板-刚度试验方法-(Taber刚度试验方法)”进行试验，通过下式算出弯矩。
弯矩(gf·cm)＝(刻度的读数)×38.0(mm)÷(测定的试验片的宽度：mm)
[树脂密合性]
在下述形状保持性试验中，观察弯曲加工评价后的试验片，通过目测观察发泡粘接剂层是否部分从耐热基材脱落。
[形状保持性]
如图9所示，在L字型铝框(板厚3mm)13上放置发泡前的试验片(粘接片14)，一边将像披萨刀(Pizza cutter)那样形状的按压夹具15从试验片14上以45度的角度朝着角部进行按压旋转，一边如图9(i)所示，按照L字型的方式对试验片14实施弯曲加工。弯曲加工后取出试验片，如图9(ii)所示，使用量角器测定5秒后的试验片14的形状。通过下式进行计算，按照以下基准评价形状保持性。
形状保持率(％)＝90度÷(弯曲加工5秒后的角度)×100(％)
“◎”：形状保持率为80％以上、100％以下
“○”：形状保持率为65％以上、小于80％
“×”：形状保持率小于65％
[发泡后厚度的均匀性]
在上述发泡后的粘接片的厚度测定的试验片中，进行10点测定，按照以下的判定基准评价相对于平均厚度的最大或最小的厚度。
“◎”：相对于平均厚度的最大或最小的厚度为5％以内。
[粘连性]
以25×80mm的大小切出2片发泡固化前的试样，在膨胀粘接剂层面的长度方向的一侧端部至15mm的位置，薄薄地擦上碳酸钙粉末，形成无粘着部(粘接面积为25×65mm)。在此之后，将在该面贴合有试样的脱模剂层的试验片夹入2张不锈钢板中，施加1kg的载荷，于40℃放置336小时后取出，于室温冷却2小时后，进行剥离使试验片分开，按照以下的基准评价粘连的程度。
“◎”：粘接面的两面都有光泽，完全未融合。
[表3]
表3
[表4]
表4
[表5]
表5
＜评价＞
由表3所示的结果可知：实施例1～10的粘接片所有物性都优异。具体而言，在初期，粘接强度以及电绝缘性优异。另外，具有适当的片强度和弯曲后的形状保持性，作业性优异。而且，通过在粘接剂层的表面涂布脱模剂，能够形成不一定需要使用剥离纸的构成。另外实施例11的粘接片在初期的粘接强度也优异。
另一方面，比较例1以及2的粘接片由于使用了未包含酚醛树脂T1的粘接剂(配合3)作为用于形成膨胀性粘接剂层的粘接剂，因此剪切粘接力差。
参考例1～3以及比较例1的粘接片的强度(刚度)以及形状保持性差。这可认为是因为使用了作为薄单层膜的基材K8～K10(另外，在实施例10中也使用了作为薄单层膜的基材K8，但由于在实施例10中在膨胀性粘接剂层中使用了包含玻璃纤维的粘接剂(配合7)，因此强度(刚度)以及形状保持性不会产生问题)。其中参考例1～3的粘接片由于使用了包含酚醛树脂T1的粘接剂(配合2或6)作为用于形成膨胀性粘接剂层的粘接剂，因此与比较例1以及2相比，剪切粘接力优异。因此，可以说在参考例1～3中也表现了本发明的效果。
工业实用性
本发明的粘接片尽管短时间发泡固化，但柔软性、电绝缘性、耐热性以及粘接性仍然优异。因此，例如在为了被粘接构件间的粘接以及绝缘而使膨胀性粘接剂层发泡固化并填埋被粘接构件间的间隙的用途中有用。特别是适宜用于马达槽的粘接绝缘用。具体而言，用于电动发电机中的定子与线圈那样的2个构件间，通过加热进行发泡、膨胀，填充该间隙而能够将构件彼此粘接。
符号说明
1 基材
2 膨胀性粘接剂层
3 脱模剂层
4 膜
5 贴合用粘接剂层
6 无纺布
7 纸
8 功能性粘接剂层
9 剥离膜
10 粘接片
11 SPCC板
12 金属塞尺
13 L字型铝框
14 粘接片
15 按压夹具

Claims (26)

1.一种粘接片，其具有膨胀性粘接剂层，所述膨胀性粘接剂层含有包含多官能环氧树脂的环氧树脂、作为固化剂的酚醛树脂、作为固化催化剂的咪唑系化合物、以及温敏性发泡剂。
2.根据权利要求1所述的粘接片，温敏性发泡剂包含热膨胀性微胶囊，该热膨胀性微胶囊的发泡温度为环氧树脂的软化点以上、且环氧树脂的固化反应的活化温度以下。
3.根据权利要求1所述的粘接片，膨胀性粘接剂层中作为固化剂的酚醛树脂的羟基当量数相对于环氧树脂的环氧当量数的比率为0.5～2.0。
4.根据权利要求1所述的粘接片，咪唑系化合物的含量相对于膨胀性粘接剂层中的树脂成分100质量份为0.1～1.0质量份。
5.根据权利要求1所述的粘接片，温敏性发泡剂的含量相对于膨胀性粘接剂层中的树脂成分100质量份为0.5～20质量份。
6.根据权利要求1所述的粘接片，膨胀性粘接剂层进一步包含聚氨酯树脂。
7.根据权利要求1所述的粘接片，在基材的一面或两面具有膨胀性粘接剂层。
8.根据权利要求7所述的粘接片，基材由具有层叠结构的层叠体构成，所述层叠结构通过利用贴合用粘接剂将树脂膜与无纺布、或树脂膜与纸、或树脂膜与树脂膜贴合而成。
9.根据权利要求8所述的粘接片，膨胀性粘接剂层或贴合用粘接剂包含耐热性填料。
10.根据权利要求8所述的粘接片，膨胀性粘接剂层或贴合用粘接剂包含纤维状填料。
11.根据权利要求7所述的粘接片，基材由在选自由树脂膜、无纺布和纸组成的组中的构件的一面或两面具有功能性粘接剂层的层叠体构成。
12.根据权利要求11所述的粘接片，膨胀性粘接剂层或功能性粘接剂层包含耐热性填料。
13.根据权利要求11所述的粘接片，膨胀性粘接剂层或功能性粘接剂层包含纤维状填料。
14.根据权利要求10或13所述的粘接片，纤维状填料为玻璃纤维，该玻璃纤维的平均纤维直径为1～20μm，平均纤维长度为10～200μm。
15.根据权利要求8所述的粘接片，无纺布为选自由芳族聚酰胺纤维无纺布、玻璃纤维无纺布、聚苯硫醚纤维无纺布、耐热尼龙纤维无纺布和耐热聚酯纤维无纺布组成的组中的一种以上无纺布。
16.根据权利要求8所述的粘接片，纸为由全芳香族聚酰胺聚合物构成的高耐热性纸。
17.根据权利要求1所述的粘接片，在至少一个膨胀性粘接剂层的表面涂布有脱模剂。
18.根据权利要求17所述的粘接片，在基材的两面具有膨胀性粘接剂层，在至少一个该膨胀性粘接剂层的表面涂布有脱模剂。
19.根据权利要求17所述的粘接片，脱模剂为长链烷基系化合物。
20.根据权利要求1所述的粘接片，膨胀性粘接剂层发泡固化后的粘接片依照JIS Z1541的剪切粘接力在室温(23℃)时为200N/cm2以上，在200℃加热时为50N/cm2以上。
21.根据权利要求1所述的粘接片，膨胀性粘接剂层发泡固化后的粘接片依照JIS C2107的绝缘击穿电压为10kV以上，热导率为0.1W/mK以上。
22.根据权利要求1所述的粘接片，膨胀性粘接剂层发泡固化前的粘接片依照JIS P8125的弯矩为40～600gf·cm。
23.根据权利要求1所述的粘接片，膨胀性粘接剂层发泡固化前的粘接片通过以下方法测定的形状保持率为70％以上，
形状保持率
在L字型铝框上放置膨胀性粘接剂层发泡固化前的粘接片，将按压夹具从粘接片的上面以45度的角度朝着角部进行按压，按照成为L字型的方式施加弯曲加工，取出试验片，测定5秒后试验片弯曲部分的角度，通过下式进行计算，
形状保持率(％)＝90度÷(弯曲加工5秒后的角度)×100(％)。
24.根据权利要求1所述的粘接片，膨胀性粘接剂层进行发泡固化前的粘接片的厚度为250μm以下。
25.根据权利要求1所述的粘接片，用于为了进行被粘接构件间的粘接和绝缘而使膨胀性粘接剂层发泡固化并填埋该被粘接构件间的间隙的用途中。
26.根据权利要求25所述的粘接片，用于马达槽的粘接绝缘用。
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