CN106457801A - 导热性片和导热性片的制备方法 - Google Patents
导热性片和导热性片的制备方法 Download PDFInfo
- Publication number
- CN106457801A CN106457801A CN201580017182.6A CN201580017182A CN106457801A CN 106457801 A CN106457801 A CN 106457801A CN 201580017182 A CN201580017182 A CN 201580017182A CN 106457801 A CN106457801 A CN 106457801A
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- China
- Prior art keywords
- heat conductivity
- block copolymer
- styrene
- polyvinyl acetal
- ethylene base
- 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.)
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Abstract
本发明提供丙烯酸类树脂层与支撑片的密合性优异的导热性片及其制备方法。导热性片具有:由丙烯酸类导热组合物形成的导热树脂层(11);以及,含有聚乙烯醇缩醛树脂和苯乙烯‑乙烯基异戊二烯嵌段共聚物的支撑树脂层(支撑片)(12)。由于支撑片与丙烯酸类导热树脂层的丙烯酸单体交联,因此可提高导热树脂层与支撑片的密合性。
Description
技术领域
本发明涉及用于电子部件等的散热对策的丙烯酸类的导热性片和导热性片的制备方法。本申请是以在日本国内2014年3月31日所申请的日本专利申请编号特愿2014-74776为基础而要求优先权的申请,该申请通过参照而引用到本申请中。
背景技术
近年来,为了电子部件等的散热对策而使用导热性片(例如,参见专利文献1)。在导热性片中,为了提高与电子部件的密合性,有时使用具有优异的柔软性的导热树脂层,但具有优异的柔软性的导热树脂层在使用时会可能会伸长或断裂,因而难以操作。因此,使用补强导热树脂层的支撑片。
但是,作为支撑片,例如使用PET膜时,丙烯酸类的导热树脂层可简单地被剥离。因此,有必要对PET膜进行底涂处理,导致工序数增加。
现有技术文献
专利文献
专利文献1:日本特开2007-123624号公报。
发明内容
发明所要解决的课题
本发明鉴于上述现有的实情而提出,提供丙烯酸类树脂层与支撑片的密合性优异的导热性片及其制备方法。
用于解决课题的手段
本发明人进行了深入的研究,结果发现了:通过使用含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑片,提高丙烯酸类树脂层与支撑片的密合性。
即,本发明的导热性片,其特征在于具有:由丙烯酸类导热组合物形成的导热树脂层;以及,含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑树脂层。
另外,本发明的支撑片,其特征在于含有:聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物。
另外,本发明的导热性片的制备方法,其特征在于具有下述的工序:将聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物混合,进行片状化,形成支撑树脂层的工序;以及,使丙烯酸类导热组合物在与上述支撑树脂层接触的状态下固化,形成导热树脂层的工序。
另外,本发明的支撑片的制备方法,其特征在于:将聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物混合,进行片状化。
发明效果
根据本发明,由于含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑树脂层与丙烯酸类树脂层的丙烯酸单体交联,因此可提高丙烯酸类树脂层与支撑片的密合性。
附图说明
[图1]图1是显示本发明的一个实施方式的导热性片的一个例子的截面图。
[图2]图2是导热树脂层与支撑树脂层的T型剥离强度的测定方法的说明图。
具体实施方式
下面,对于本发明的实施方式,参见附图的同时按照下述的顺序进行详细说明。
1. 导热性片
2. 导热性片的制备方法
3. 实施例
<1. 导热性片>
本发明的一个实施方式的导热性片具备:由丙烯酸类导热组合物形成的导热树脂层;以及,含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑树脂层。导热性片的优选厚度为0.1mm以上且10.0mm以下,支撑树脂层的优选厚度为0.001mm以上且0.500mm以下。
图1是显示本发明的一个实施方式的导热性片的一个例子的截面图。该导热性片具备:使丙烯酸类导热组合物固化而形成的导热树脂层11;以及,支撑导热树脂层11的支撑树脂层12。另外,导热树脂层11的面上贴合有在使用时被剥离的剥离膜13。
导热树脂层11是丙烯酸类导热组合物固化而得的层。导热树脂层11的优选导热率为0.3W/m·K以上。另外,导热树脂层11的载荷1kgf/cm2时的优选压缩率为1%以上且80%以下。压缩率越高,柔软性越优异,对于发热体或散热体可获得优异的密合性。另外,导热树脂层11的优选阿斯卡C硬度(ASKER C 硬度,JISK 7312)为5以上且60以下。
作为丙烯酸类导热组合物,可使用以往公知的丙烯酸类导热组合物。例如可举出:含有(A)单官能(甲基)丙烯酸酯、(B)多官能(甲基)丙烯酸酯、(C)光聚合引发剂、(D)导热性粒子、(E)增塑剂、以及(F)硫醇化合物的丙烯酸类导热组合物。
作为单官能(甲基)丙烯酸酯,优选使用具有直链或支链烷基的(甲基)丙烯酸烷基酯。作为(甲基)丙烯酸烷基酯,例如可举出:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丙酯、(甲基)丙烯酸异丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸仲丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸正己酯、丙烯酸环己酯、(甲基)丙烯酸正庚酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正壬酯、(甲基)丙烯酸异壬酯、(甲基)丙烯酸正癸酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸正十二烷基酯、(甲基)丙烯酸异肉豆蔻基酯、(甲基)丙烯酸正十三烷基酯、(甲基)丙烯酸正十四烷基酯、(甲基)丙烯酸正十八烷基酯、(甲基)丙烯酸异十八烷基酯、(甲基)丙烯酸正月桂基酯等,可使用这些的1种或2种以上。
作为多官能(甲基)丙烯酸酯,例如可举出: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、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、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、三丙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯等双官能的(甲基)丙烯酸酯;三羟甲基丙烷三(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、三(丙烯酰氧基乙基)异氰尿酸酯、二-三羟甲基丙烷四(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二季戊四醇单羟基五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯等三官能以上的(甲基)丙烯酸酯,可使用这些的1种或2种以上。
作为光聚合引发剂,可举出:二苯甲酮类、苯偶姻类、苯偶姻烷基醚类、苯偶酰二甲基缩酮类、α-羟基酮类、酰基氧化膦类等,可使用这些的1种或2种以上。
作为导热性粒子,可举出:氢氧化铝、氢氧化镁等金属氢氧化物;铝、铜、银等金属;氧化铝、氧化镁等金属氧化物;氮化铝、氮化硼、氮化硅等氮化物;碳纳米管等,可使用这些的1种或2种以上。
关于导热性粒子在丙烯酸类导热组合物中的含量,相对于100质量份的单官能(甲基)丙烯酸酯,为100质量份以上且2000质量份、优选为300质量份以上且650质量份以下。若导热性粒子的含量过少,则导热性片的导热性难以充分提高,若导热性粒子的含量过多,则导热性片的柔软性存在降低的倾向。另外,在使用平均粒径不同的2种导热性填料时,优选小直径填料与大直径填料的掺混比为15:85~90:10。
作为增塑剂,例如可使用选自下述的至少1种:己二酸酯、庚二酸酯、辛二酸酯、壬二酸酯、癸二酸酯。这样的二羧酸酯可通过将选自己二酸(HOOC-(CH2)4-COOH)、庚二酸(HOOC-(CH2)5-COOH)、辛二酸(HOOC-(CH2)6-COOH)、壬二酸(HOOC-(CH2)7-COOH)、癸二酸(HOOC-(CH2)8-COOH)的二羧酸和醇由常规方法进行酯化而获得。作为更具体的增塑剂,优选使用选自下述的至少1种:将选自己二酸、庚二酸、辛二酸、壬二酸、癸二酸的1种和异癸醇进行酯化而得的己二酸二异癸酯、庚二酸二异癸酯、辛二酸二异癸酯、壬二酸二异癸酯、癸二酸二异癸酯。
作为硫醇化合物,使用双官能以上的多官能硫醇。作为双官能以上的多官能硫醇,可举出:1,3,5-三(3-巯基丁基氧基乙基)-1,3,5-三嗪-2,4,6(1H,3H,5H)-三酮、2-甲基-2-((3-巯基-1-氧代丙基)-甲基)丙烷-1,3-二基双(3-巯基丙酸酯)、三羟甲基丙烷三硫代丙酸酯、三羟甲基丙烷三硫代乙二醇、2,4,6-三巯基-S-三嗪等三官能硫醇化合物;季戊四醇四(3-巯基丁酸酯)、季戊四醇四硫代乙醇酸酯、二季戊四醇四硫代乙醇酸酯、季戊四醇四硫代丙酸酯等四官能硫醇化合物;二季戊四醇五硫代乙醇酸酯等五官能硫醇化合物;二季戊四醇六硫代乙醇酸酯等六官能硫醇化合物等,可使用这些的1种或2种以上。
另外,在丙烯酸类导热组合物中,作为其它成分,可掺混抗氧化剂、防热老化剂、阻燃剂、着色剂等。
作为抗氧化剂,可举出:捕捉因热老化而产生的自由基的抗一次氧化剂、分解因热老化而产生的过氧化物的抗二次氧化剂等,这些可单独使用也可将2种以上并用。作为防热老化剂,可举出:1,1-双(2-羟基-3,5-二-叔戊基苯基)甲烷的丙烯酸单酯。
另外,关于丙烯酸类导热组合物,不限于上述的构成,还可使用其它丙烯酸类导热组合物。例如,作为市售品,可举出:TransCool(トランスクール)系列GNS((株) INOACCORPORATION)、シロキノン系列((株)Taica)、5580H(住友3M (株))等。
支撑树脂层12是含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑片。
聚乙烯醇缩醛树脂是将聚乙烯醇通过醛进行缩醛化而得的树脂。关于聚乙烯醇,例如可通过将聚醋酸乙烯酯进行皂化而获得,其皂化度通常为80摩尔%以上且99.8摩尔%以下。另外,聚乙烯醇的聚合度通常为200以上且3000以下。作为醛,可举出:甲醛、乙醛、正丁醛、异丁醛、正己醛、正戊醛等,可使用这些的1种或2种以上。其中,适合使用使乙醛或丁醛与聚乙烯醇反应而获得的聚乙烯醇缩乙醛或聚乙烯醇缩丁醛。
聚乙烯醇缩醛树脂的分子量为5×104以上且20×104以下,更优选为8×104以上且15×104以下。若分子量过低,则表现出粘性,支撑片的干燥性有可能降低,若分子量过高,则支撑片的柔软性有可能降低。
另外,聚乙烯醇缩醛树脂的玻璃化转变温度(Tg)为50℃以上且150℃以下,更优选为80℃以上且120℃以下。若玻璃化转变温度过低,则表现出粘性,支撑片的干燥性有可能降低,若玻璃化转变温度过高,则支撑片的柔软性有可能降低。
另外,聚乙烯醇缩醛树脂的缩醛化度(为聚乙烯醇缩丁醛树脂时,指丁缩醛化度)为50摩尔%以上且90摩尔%以下,更优选为60摩尔%以上且80摩尔%以下。若缩醛化度过低,则与苯乙烯-乙烯基异戊二烯嵌段共聚物的相容性有可能降低,若缩醛化度过高,则支撑片的耐热性有可能降低。
缩醛化度是将缩醛基所键合的乙烯基量除以主链的总乙烯基量而求得的摩尔分率以百分率表示的值。缩醛化度可如下算出:利用基于JIS K6728“聚乙烯醇缩丁醛试验方法”的方法,测定乙酰化度(乙酰基量)和羟基的含有率(乙烯基醇量),根据所得的测定结果算出摩尔分率,接着,从100摩尔%中减去乙酰化度和羟基的含有率,由此而算出。
作为这样的聚乙烯醇缩醛树脂的市售品,例如可举出:S-LEC BX-1、BX-5、KS-3、KS-5(积水化学(株))等。
苯乙烯-乙烯基异戊二烯嵌段共聚物是由苯乙烯嵌段和乙烯基-聚异戊二烯嵌段构成的三嵌段共聚物,是将苯乙烯单元作为硬链段、乙烯基异戊二烯单元作为软链段的热塑性弹性体。
苯乙烯-乙烯基异戊二烯嵌段共聚物的苯乙烯含量为10%以上且30%以下,优选为15%以上且25%以下。若苯乙烯含量过少,则硬链段不充分,橡胶弹性有可能降低,若苯乙烯含量过多,则支撑片的柔软性有可能降低。
另外,苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度(Tg)为-40℃以上且+40℃以下,优选为-20℃以上且+20℃以下。若玻璃化转变温度过低,则表现出粘性,支撑片的干燥性有可能降低,若玻璃化转变温度过高,则支撑片的柔软性有可能降低。
作为这样的苯乙烯-乙烯基异戊二烯嵌段共聚物的市售品,例如可举出:HYBRAR5125、5127((株)Kuraray)等。
另外,优选聚乙烯醇缩醛与苯乙烯-乙烯基异戊二烯嵌段共聚物以9:1~7:3的质量比例进行掺混。若苯乙烯-乙烯基异戊二烯嵌段共聚物的掺混量过少,则无法获得与导热树脂层的密合性,若苯乙烯-乙烯基异戊二烯嵌段共聚物的掺混量过多,则有可能导致支撑片的干燥性降低或强度降低。
另外,在支撑树脂层12中可添加交联剂。作为交联剂,可举出:异氰酸酯类交联剂、环氧类交联剂、有机硅类交联剂等,可使用这些的1种或2种以上。
另外,优选支撑树脂层12的表面粗糙。通过使支撑树脂层12的表面粗糙,而使其与导热性树脂接触的表面积增加,从而增加乙烯基的交联点,因此可通过固着效果来提高密合性。
作为剥离膜13,例如可使用:将有机硅等的剥离剂涂布于PET(PolyethyleneTerephthalate,聚对苯二甲酸乙二醇酯)、OPP(Oriented Polypropylene,取向聚丙烯)、PMP(Poly-4-methylpentene-1,聚-4-甲基戊烯-1)、PTFE(Polytetrafluoroethylene,聚四氟乙烯)等而形成的膜。
根据这样的导热性片,由于含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑树脂层与丙烯酸类的导热树脂层的丙烯酸单体进行交联,因此可提高导热树脂层与支撑片的密合性。另外,由于支撑片的表面干燥,因此可提高操作性。另外,由于导热性片的导热性和柔软性优异,因此可适合用于硬盘装置、激光装置等的精密仪器。
需要说明的是,在上述的实施方式中,虽然制成了在导热树脂层的单面上设置支撑树脂层的构成,但也可制成在导热树脂层的双面上设置支撑树脂层的构成,也可制成在支撑树脂层的双面上设置导热树脂层的构成。另外,在上述的实施方式中,将支撑片应用于导热性片,但不限于此。例如,可将支撑片用作丙烯酸类的胶粘带或粘合带的支撑材料。
<2. 导热性片的制备方法>
本发明的一个实施方式的导热性片的制备方法具有下述的工序:将聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物混合,进行片状化,形成支撑树脂层的工序;以及,使丙烯酸类导热组合物在与上述支撑树脂层接触的状态下固化,形成导热树脂层的工序。
在形成支撑树脂层的工序中,向聚乙烯醇缩醛树脂中添加并混合苯乙烯-乙烯基异戊二烯嵌段共聚物,来调制支撑树脂组合物,其中,相对于100质量份的聚乙烯醇缩醛树脂,使苯乙烯-乙烯基异戊二烯嵌段共聚物达到10质量份以上且65质量份以下、优选10质量份以上且45质量份以下。片状化可如下进行:例如,利用刮条涂布机在剥离膜上均匀地涂布支撑树脂组合物,并干燥。由于聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物为热塑性树脂,因此可使用喷射模塑法、挤出成形法、混炼法等在无溶剂下进行片状化。
在形成导热树脂层的工序中,使丙烯酸类导热组合物在与支撑树脂层接触的状态下固化。认为由此,支撑树脂层的苯乙烯-乙烯基异戊二烯嵌段共聚物的乙烯基部分和丙烯酸类导热组合物的丙烯酸单体部分相溶或固化,从而形成一体化,可提高密合性。固化方法可使用光、热、溶剂等以往的固化方法,但优选使用光或热中的至少一种。
另外,在形成导热树脂层的工序中,可使丙烯酸类导热组合物在用2个支撑片夹持的状态下固化,也可使丙烯酸类导热组合物在涂布于支撑片的双面上的状态下固化。
根据这样的导热片的制备方法,在形成导热树脂层的工序中,通过丙烯酸类导热组合物的固化,可将导热树脂层与支撑树脂层牢固地粘合。
实施例
<3. 实施例>
下面,对本发明的实施例进行说明。在本实施例中,将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以规定的质量比例混合,形成了支撑树脂层。接着,在支撑树脂层上形成使丙烯酸类导热组合物固化而得的导热树脂层,制作了导热性片。然后,对于各导热性片,测定并评价了拉伸强度、支撑树脂层与导热树脂层的T型剥离强度、以及支撑树脂层的表面粘性。需要说明的是,本发明不限于这些实施例。
导热性片的制作、拉伸强度的测定及评价、T型剥离强度的测定及评价、以及表面粘性的测定及评价如下进行。
[导热性片的制作]
将聚乙烯醇缩醛(S-LEC BX-1、积水化学(株))和苯乙烯-乙烯基异戊二烯嵌段共聚物(HYBRAR 5125、(株)Kuraray)以规定的质量比例混合,获得了支撑树脂组合物。利用刮条涂布机将该支撑树脂组合物涂布于由PET形成的剥离膜上,形成了厚度为0.01mm的支撑树脂层。
将作为单官能丙烯酸酯的丙烯酸2-乙基己酯100质量份、作为增塑剂的蓖麻油衍生脂肪酸酯47质量份、作为多官能丙烯酸酯的羟基特戊酸新戊二醇二丙烯酸酯(KAYARADFM-400、日本化药(株))1.5质量份、光聚合引发剂(IRGACURE 819、BASF(株))1.4质量份、作为导热性填料的氢氧化铝粉(平均粒径80μm)400质量份、氢氧化铝粉(平均粒径8μm)400质量份混合,调制了丙烯酸类导热组合物。
将丙烯酸类导热组合物涂布于支撑树脂层上,从丙烯酸类导热组合物面和支撑树脂层面这两侧以1mW/cm2的照射强度同时照射紫外线5分钟,在支撑树脂层上形成导热树脂层,制作了由厚度0.01mm的支撑树脂层和厚度1.0mm的导热树脂层构成的导热性片。
[拉伸强度的测定及评价]
将由导热树脂层11和支撑树脂层12构成的导热性片利用最窄宽度5mm、最窄部的长度20mm的冲孔模(哑铃状3号)、使用手动压力机进行加工,制作了试样。将该试样利用拉伸试验机(RTG-1225、Orientec公司)、以速度500mm/分钟进行拉伸,测定了断开(断裂)时的强度(将拉伸载荷值除以试验片的截面积而得的值)。将拉伸强度为0.4MPa以上的试样评价为“○”,不足0.4MPa的试样评价为“×”。
[T型剥离强度的测定及评价]
利用拉伸试验机(RTG-1225、Orientec公司),如图2所示,在导热树脂层11上贴合由PET构成的剥离膜13A、在支撑树脂层12上贴合由PET构成的剥离膜13B,在该状态下,通过T型剥离试验测定了导热树脂层11与支撑树脂层12的层间剥离强度。此时的拉伸速度为300mm/分钟、试样宽度为15mm。将层间剥离强度为0.2N/20mm以上的试样评价为“○”、不足0.2N/20mm且为0.15N/20mm以上的试样评价为“△”、以及不足0.15N/20mm的试样评价为“×”。
[表面粘性的测定及评价]
作为粘性试验机,使用了RHESCA公司制造的粘性试验机TAC-II,将直径10mm的铝制圆柱状探针在按压速度30mm/分钟、剥下速度120mm/分钟、载荷196g、按压时间5.0秒、拉伸距离5mm、探针未加热的条件下按压到支撑树脂层上,测定了剥下时的探针粘性。将支撑树脂层的粘性不足10kN/m2的试样评价为“○”、10kN/m2以上且不足15kN/m2的试样评价为“△”、以及15kN/m2以上的试样评价为“×”。
<比较例1>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以10:0的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例1的拉伸强度的评价为○、T型剥离强度的评价为×、以及表面粘性的评价为○。
<实施例1>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以9:1的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,实施例1的拉伸强度的评价为○、T型剥离强度的评价为△、以及表面粘性的评价为○。
<实施例2>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以8.5:1.5的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,实施例2的拉伸强度的评价为○、T型剥离强度的评价为○、以及表面粘性的评价为○。
<实施例3>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以8:2的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,实施例3的拉伸强度的评价为○、T型剥离强度的评价为○、以及表面粘性的评价为○。
<实施例4>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以7:3的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,实施例4的拉伸强度的评价为○、T型剥离强度的评价为○、以及表面粘性的评价为△。
<比较例2>
除了将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以0:10的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例2的拉伸强度的评价为×、T型剥离强度的评价为○、以及表面粘性的评价为×。
<比较例3>
除了将聚乙烯醇缩醛和苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(SEPTON V9827、(株)Kuraray)以9:1的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例3的拉伸强度的评价为○、T型剥离强度的评价为×、以及表面粘性的评价为○。
<比较例4>
除了将聚乙烯醇缩醛和苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(SEPTON V9827、(株)Kuraray)以7:3的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例4的拉伸强度的评价为○、T型剥离强度的评价为×、以及表面粘性的评价为○。
<比较例5>
除了将聚乙烯醇缩醛和苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(SEPTON V9827、(株)Kuraray)以3:7的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例5的拉伸强度的评价为×、T型剥离强度的评价为×、以及表面粘性的评价为×。
<比较例6>
除了将聚乙烯醇缩醛和苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物(SEPTON V9827、(株)Kuraray)以0:10的质量比例混合形成支撑树脂层以外,如上制作了导热性片。如表1所示,比较例6的拉伸强度的评价为×、T型剥离强度的评价为×、以及表面粘性的评价为×。
[表1]
如比较例3~6所示,添加不具有不饱和键的苯乙烯-乙烯/丁烯-苯乙烯嵌段共聚物时,导热树脂层与支撑树脂层的层间剥离强度小,无法获得优异的密合性。另外,如比较例1所示,为仅由聚乙烯醇缩醛形成的支撑树脂层时,导热树脂层与支撑树脂层的层间剥离强度小,无法获得优异的密合性。另外,如比较例2所示,为仅由苯乙烯-乙烯基异戊二烯嵌段共聚物形成的支撑树脂层时,导热性片的拉伸强度降低,且支撑树脂层上表现出粘性而使干燥性降低。
另一方面,如实施例1~4所示,将聚乙烯醇缩醛和苯乙烯-乙烯基异戊二烯嵌段共聚物以9:1~7:3的质量比例混合形成支撑树脂层时,导热树脂层与支撑树脂层的层间剥离强度大,可获得优异的密合性。另外,导热性片的拉伸强度也大,且还可维持支撑树脂层的干燥性。
符号说明
11 导热树脂层、12 支撑树脂层、13 剥离膜
Claims (20)
1.导热性片,该导热性片具备:
由丙烯酸类导热组合物形成的导热树脂层;以及,
含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物的支撑树脂层。
2.权利要求1所述的导热性片,其中,上述聚乙烯醇缩醛和上述苯乙烯-乙烯基异戊二烯嵌段共聚物以9:1~7:3的质量比例掺混。
3.权利要求1或2所述的导热性片,其中,上述聚乙烯醇缩醛树脂为聚乙烯醇缩乙醛或聚乙烯醇缩丁醛。
4.权利要求1或2所述的导热性片,其中,上述聚乙烯醇缩醛树脂的分子量为5×104以上且20×104以下。
5.权利要求3所述的导热性片,其中,上述聚乙烯醇缩醛树脂的分子量为5×104以上且20×104以下。
6.权利要求1或2所述的导热性片,其中,上述聚乙烯醇缩醛树脂的玻璃化转变温度为50℃以上且150℃以下。
7.权利要求3所述的导热性片,其中,上述聚乙烯醇缩醛树脂的玻璃化转变温度为50℃以上且150℃以下。
8.权利要求4所述的导热性片,其中,上述聚乙烯醇缩醛树脂的玻璃化转变温度为50℃以上且150℃以下。
9.权利要求1或2所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的苯乙烯含量为10%以上且30%以下。
10.权利要求3所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的苯乙烯含量为10%以上且30%以下。
11.权利要求4所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的苯乙烯含量为10%以上且30%以下。
12.权利要求6所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的苯乙烯含量为10%以上且30%以下。
13.权利要求1或2所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度为-40℃以上且+40℃以下。
14.权利要求3所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度为-40℃以上且+40℃以下。
15.权利要求4所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度为-40℃以上且+40℃以下。
16.权利要求6所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度为-40℃以上且+40℃以下。
17.权利要求9所述的导热性片,其中,上述苯乙烯-乙烯基异戊二烯嵌段共聚物的玻璃化转变温度为-40℃以上且+40℃以下。
18.支撑片,该支撑片含有聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物。
19.导热性片的制备方法,该方法具有下述的工序:
将聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物混合,进行片状化,形成支撑树脂层的工序;以及,
使丙烯酸类导热组合物在与上述支撑树脂层接触的状态下固化,形成导热树脂层的工序。
20.支撑片的制备方法,其中,将聚乙烯醇缩醛树脂和苯乙烯-乙烯基异戊二烯嵌段共聚物混合,进行片状化。
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