CN107033800A - 导热性薄片 - Google Patents

导热性薄片 Download PDF

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Publication number
CN107033800A
CN107033800A CN201710131494.0A CN201710131494A CN107033800A CN 107033800 A CN107033800 A CN 107033800A CN 201710131494 A CN201710131494 A CN 201710131494A CN 107033800 A CN107033800 A CN 107033800A
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Prior art keywords
thermal conductivity
thin slice
conducting layer
resin bed
adhesive resin
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Granted
Application number
CN201710131494.0A
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CN107033800B (zh
Inventor
杉田纯郎
杉田纯一郎
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Dexerials Corp
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Dexerials Corp
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    • 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
    • C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
    • C09J133/04—Homopolymers or copolymers of esters
    • C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09J133/08—Homopolymers or copolymers of acrylic acid esters
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin 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
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    • B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
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  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
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  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Nanotechnology (AREA)
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Abstract

本发明的目的是通过使导热性薄片的一个面形成适度粘附性来提高导热性薄片的加工性和再加工性。导热性薄片层叠有粘附性导热层和非粘附性树脂层。粘附性导热层含有丙烯酸类树脂和导热性填料，丙烯酸类树脂的玻璃化转变温度为‑80至15℃，并且粘附性导热层的粘性高于非粘附性树脂层的粘性，非粘附性树脂层的玻璃化转变温度为60到110℃。该非粘附性树脂层的探针粘附力为6至30kN/m2。或者，非粘附性树脂层与粘附性导热层之间的T型剥离强度在0.2N/cm以上。

Description

导热性薄片
本申请是2014年3月26日递交的申请号为201480013296.9，发明名称为“导热性薄片”的分案申请。
技术领域
本发明涉及一种粘贴至电子部件提高电子部件的散射性的导热性薄片。
背景技术
导热性薄片用于填充成为发热源的电子部件等与散热板、壳体等的散热器之间的间隙，以用于提高电子部件的散热性。作为导热性薄片，从使用其组装电子部件和散热器时的加工性的观点来看，优选具有粘附性。进一步，从校正电子部件和散热器在组装时的位置偏移，以及能够在组装后因某事进行拆卸并再次组装等的再加工性的观点来看，优选提高一个面的粘附性，降低另一个面的粘附性。
因此，(专利文献1)提出如下方案：在用硅橡胶和导热性填料形成导热性薄片时，利用紫外线照射对导热性薄片的表面实施非粘附处理。
此外，(专利文献2)提出如下方案：含有无官能性丙烯酸聚合物和导热性填料的丙烯酸类聚氨酯树脂的粘附性导热性薄片中，通过在正面层和背面层使丙烯酸类聚氨酯树脂与无官能丙烯酸聚合物的配合比不同并重复涂覆至各层，从而使粘附性导热性薄片的正背的粘附性不同。
现有技术文献
专利文献
专利文献1：日本专利公报第3498823号
专利文献2：日本专利公开公报第2010-93077号
然而，如专利文献1所述，在为了降低导热性薄片的一个面的粘附性而执行紫外线照射时，承担导热的层会劣化。
此外，如专利文献2所述，在正面层和背面层使丙烯酸类聚氨酯树脂和无官能性丙烯酸聚合物的配合比不同并重叠涂覆的情况下，由于正面层和背面层容易混杂，因此难以按照所期望那样改变正面层和背面层的粘附性。
此外，作为使导热性薄片的正背的粘附性不同的方法，在由丙烯酸类树脂和导热填料形成粘附性导热层时，虽然考虑了对导热性薄片的一个面层叠非粘附性薄膜的方法，但在该情况下，由于薄膜面粘附至物体的粘附性急剧下降，因此作为导热性薄片的加工性劣化。
发明内容
针对此问题，本发明的目的在于，对于粘附性导热层由丙烯酸类树脂和导热性填料形成的导热性薄片，在粘附性导热层中的一个面形成粘附性比该粘附性导热层较低但具有适度粘附性的层，以提高导热性薄片的加工性和再加工性。
本发明人发现，能够通过以下方法实现上述目的：在由丙烯酸类树脂和导热性填料形成的粘附性导热层中的一个面层叠非粘附性树脂层的导热性薄片中，通过使非粘附性树脂层的粘性比该粘附性导热层的粘性较低且使该非粘附性树脂层的探针粘附力在特定的范围内，或者使非粘附性树脂层与粘附性导热层的剥离强度在特定的范围内，从而完成本发明。
换言之，本发明提供一种粘附性导热层和非粘附性树脂层层叠的导热性薄片，所述导热性薄片的特征在于，
粘附性导热层含有丙烯酸类化合物固化后的丙烯酸类树脂以及导热性填料，该丙烯酸类树脂的玻璃化转变温度为-80至15℃之间，粘附性导热层的粘性高于所述非粘附性树脂层的粘性，
非粘附性树脂层的玻璃化转变温度为60至110℃，
非粘附性树脂层的粘性作为通过在按压速度30mm/min、剥离速度120mm/min、负荷196g、按压时间5.0秒、拉伸距离5mm、探针加热至40℃、薄片台加热至40℃的条件下将铝制圆柱状探针按压至该非粘附性树脂层并剥离而被测定的探针粘附力为6至30kN/m2。
此外，本发明提供一种粘附性导热层和非粘附性树脂层层叠导热性薄片，所述导热性薄片的特征在于，
粘附性导热层含有丙烯酸类化合物固化后的丙烯酸类树脂以及导热性填料，该丙烯酸类树脂的玻璃化转变温度为-80至15℃之间，粘附性导热层的粘性高于非粘附性树脂层的粘性，
非粘附性树脂层的玻璃化转变温度为60至110℃，
非粘附性树脂层和粘附性导热层的T型剥离强度为0.2N/cm以上。
有益效果
根据本发明的导热性薄片，由于层叠有粘附性导热层以及比该粘附性导热层的粘性低并具有特定大小粘性的非粘附性树脂层，因此，提高了使用导热性薄片组装电子部件和散热器时的加工性，并且也提高了对组装物体重新组装的再加工性。
附图说明
图1为非粘附性树脂层与粘附性导热层之间的T型剥离强度的测定方法的说明图。
具体实施方式
以下对本发明进行详细地说明。
在本发明的导热性薄片中层叠有粘附性导热层和非粘附性树脂层。
在粘附性导热层中，丙烯酸类化合物固化后的丙烯酸类树脂中分散有导热性填料。在本发明中，从提高使用导热性薄片组装电子部件和散热器时的加工性以及对组装物体进行重新组装的再加工性的观点来看，作为丙烯酸类化合物，使用作为其固化物的丙烯酸类树脂的玻璃化转变温度为-80到15、优选的-70到-10的丙烯酸类化合物。作为这种丙烯酸类化合物，能够列举出2-乙基己基、月桂基、正丁基、异丁基、异壬基、2-羟乙基、4-羟丁基等单官能(甲基)丙烯酸酯等，其中，优选丙烯酸-2-乙基己酯、丙烯酸月桂酯。此外，能够混合使用一种以上与丙烯酸化合物可发生共聚作用的(甲基)丙烯酸、N-乙烯基吡咯烷酮、衣康酸、四氢糠基丙烯酸酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸-2-羟乙酯、(甲基)丙烯酸-2-羟丙酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸乙氧基乙酯、(甲基)丙烯酸丁氧基乙酯、(甲基)丙烯酸苯氧基乙酯、(甲基)丙烯酸苯酯、(甲基)丙烯酸环己酯等。
此外，作为丙烯酸类化合物的固化方法，例如能够为使用光聚合引发剂、光交联剂，照射紫外线的方法。在该情况下，仅照射使光聚合引发剂开裂所需能量的量的长波长紫外线(波长320至400nm)，因而不会出现粘附性导热层由于紫外线照射而劣化的问题。
作为粘附性导热层含有的导热性填料，能够使用氢氧化铝、氢氧化镁等金属氢氧化物；铝、钢、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。此外，导热性填料的平均粒径优选的为0.5至100μm，具体地，从分散性和导热性的观点来看，优选并用平均粒径为3至20μm的小直径的填料和平均粒径为25至100μm的大直径的填料。
粘附性导热层中导热性填料的含量相对于上述丙烯酸类化合物的单体单元100质量份，优选100至200质量份，更优选300至1000质量份。导热性填料的含量过少，则不能充分提高导热性薄片的导热性，相反如果过多，则导热性薄片的柔软性降低，因而均不优选。
在粘附性导热层使用平均粒径不同的两种导热性填料的情况下，优选小直径填料和大直径填料的配合比为15：85至90：10。
此外，粘附性导热层优选含有一种以上选自丙烯酸类化合物、低分子量丙烯酸聚合物、蜡和增粘剂等中的增塑剂，所述丙烯酸类化合物为含有一种以上选自由己二酸二辛酯、己二酸二异壬酯等己二酸类化合物、癸二酸辛酯、癸二酸二异癸酯等癸二酸类化合物、磷酸三甲苯酯等磷酸类化合物、蓖麻油或其衍生物、硬脂酸、油酸等高级脂肪酸和衍生物、邻苯二甲酸二丁酯、邻苯二甲酸二辛酯等邻苯二甲酸类化合物、丙烯酸丁酯、丙烯酸-2-乙基己酯、丙烯酸-2-甲氧基乙酯组成的组中的单体而成的均聚物或共聚物、或者上述单体与选自由α-烯烃、乙烯基酯、乙烯基醚的单体组成的组中的单体的共聚物等，更优选含有一种以上选自由己二酸类、癸二酸类、磷酸类、蓖麻油类、油酸类和丙烯酸类中的增塑剂。粘附性导热层中增塑剂的含量相对于上述丙烯酸类化合物的单体单元100质量份，优选20至80质量份，更优选30至70质量份。
此外，根据需要，粘附性导热层能够混合抗氧化剂、防热劣化剂、阻燃剂、着色剂等。
粘附性导热层的层厚度优选的是200至3000μm。过薄时，得不到对被粘物的凹凸的充分适应性，在过厚时，固化需要较长时间会导致生产率降低。
粘附性导热层和非粘附性树脂层的粘性是在按压速度30mm/min、剥离速度120mm/min、负荷196g、按压时间5.0秒、拉伸距离5mm、探针加热至40℃、薄片台加热至40℃的条件下将铝制圆柱状探针按压至粘附性导热层或非粘附性树脂层并剥离而作为探针粘附力进行测定的粘性。
粘附性导热层的粘性需要高于非粘附性树脂层的粘性。
在第一实施方式中，非粘附性树脂层的粘性作为探针粘附力为6到30kN/m2，优选7到25kN/m2。
此外，该非粘附性树脂层与粘附性导热层之间的粘接强度小可能带来在加工时、再加工时的操作期间的层间剥离等问题。在第二实施方式中，为了适于操作性，T型剥离强度需要在0.2N/cm以上，优选能够在0.2至6N/cm之间。
非粘附性树脂层的粘性如上述形成为具有特定范围的探针粘性且非粘附性树脂层与粘附性导热层之间的剥离强度在特定的大小以上时，非粘附性树脂层在使用导热性薄片组装电子部件和散热器时虽不粘连，但仍适度发挥低粘附性，由于提高了加工性的同时也提高对组装的物体进行重新组装时的再加工性，因而是优选的。
由于使非粘附性树脂层的粘性为上述范围，因此形成非粘附性树脂层的树脂的玻璃化转变温度的下限为60℃以上，更优选的是70℃以上。这样，不用在形成非粘附性树脂层的树脂中配合固化剂实施固化处理而能够使非粘附性树脂层的探针粘附力为30kN/m2以下，具体为25kN/m2以下。
另一方面，关于形成非粘附性树脂层的树脂的玻璃化转变温度的上限，从使非粘附性树脂层适度发挥低粘附性并获得与粘附性导热层的粘接强度的观点来看，为110℃以下。
此外，形成非粘附性树脂层的树脂优选为与形成粘附性导热层的丙烯酸类化合物不相溶。以此方式，即使重复涂覆形成各层的涂装用组合物以形成粘附性导热层和非粘附性树脂层的层叠物，各层亦难以在其界面处混杂，从而能够得到预期的粘性。与此相对，在形成非粘附性树脂层的树脂与形成粘附性导热层的丙烯酸类化合物相溶的情况下，在重复涂覆之前，通过预先对形成非粘附性树脂层的涂装层实施固化处理，各层在其界面处也难以混杂，从而能够得到预期的粘性。
作为用于形成非粘附性树脂层的优选树脂，即玻璃化转变温度为60至110℃，与形成粘附性导热层的丙烯酸类化合物不相溶的树脂，能够列举出聚乙烯醇缩丁醛树脂、聚酯树脂、聚氨酯树脂等。此外，这些树脂的分子量以数均分子量表示优选为10000至500000。
根据需要，非粘附性树脂层能够含有形成非粘附性树脂层的树脂的固化剂、氰尿酸三聚氰胺等有机类阻燃剂、氢氧化铝等导热性填料、着色剂。
非粘附性树脂层的厚度优选为0.5至25μm，更优选的为1至20μm。非粘附性树脂层的厚度过薄时，由于与粘附性导热层的相溶以及通过导热性填料的摩擦损坏而使粘附性增大，而过厚时作为导热性薄片的导热性会不充分。
现在，作为导热性薄片的导热性，实际应用中，导热性薄片在厚度方向上的导热率通过基于ASTM D5470的热倾斜法进行的测定，需要在1W/m·K以上，根据本发明能够在1.5W/m·K以上，更优选的在2W/m·K以上。
作为本发明的导热性薄片的制造方法，例如，能够通过以下方法得到本发明的导热性薄片：预先分别调制混合了形成前述粘附性导热层的各成分的粘附性导热层形成用涂料以及将形成非粘附性树脂层的各成分与溶剂混合后的非粘附性树脂层形成用涂料，在由PET、PEN、聚烯烃、玻璃纸等形成的剥离膜上涂覆非粘附性树脂层形成用涂料并干燥，随后，在此非粘附性树脂层的涂装面上重复涂覆粘附性导热层形成用涂料，在粘附性导热层形成用涂料的涂覆面上覆盖PET、PEN、聚烯烃等的覆盖膜，从上照射紫外线以固化粘附性导热层形成用涂料的涂覆层。
此外，也可以通过以下的方法制造本发明的导热性薄片：在剥离膜上涂覆非粘附性树脂层形成用涂料并干燥，另一方面在别的剥离膜上涂覆粘附性导热层形成用涂料，使与先前的非粘附性树脂层的涂装面相对覆盖以代替覆盖膜，照射紫外线以固化粘附性导热层形成用涂料的涂覆层。
现在，在以此方式制造导热性薄片后，能够剥离非粘附性树脂层并将导热性薄片卷绕进行保管。以此方式卷绕的导热性薄片剥离粘附性导热层侧的剥离膜以用于电子部件与散热器的组装。
实施例
以下，根据实施例对本发明进行具体地说明。
实施例1至7、比较例1至3
将表1中示出的树脂和固化剂在甲苯:甲乙酮＝1:1的混合溶剂中调制成固含量为10质量％，通过刮条涂布机涂覆至PET膜，在90℃干燥5分钟，从而形成表1中示出的涂覆厚度的非粘附性树脂层。
另一方面，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、光聚合引发剂(Irgacure 819、BASF)1.4质量份、作为固化剂的羟基三甲基乙酸新戊二醇二丙烯酸酯(KAYARAD FM-400日本化药)1.5质量份、作为导热性填料的氢氧化铝粉末(平均粒径80μm)400质量份、氢氧化铝粉末(平均粒径8μm)400质量份混合以调制粘附性导热层形成用涂料。而且，该丙烯酸-2-乙基己酯的固化物的玻璃化转变温度为-50至-40℃。
将以此方式调制的粘附性导热层形成用涂料以2mm涂层厚度重复涂覆至上述的非粘附性树脂层上，在其上覆盖由PET制成的覆盖膜，从PET膜侧和覆盖膜侧的两侧用化学灯照射5分钟长波长紫外线，从而制造出实施例1至7以及比较例1至3的导热性薄片。
比较例4
将与实施例1同样调制的粘附性导热层在没有设置非粘附性树脂层的情况下涂覆至PET膜，在其上覆盖由PET制成的覆盖膜，从PET膜侧和覆盖膜侧的两侧用化学灯照射5分钟，从而制造出比较例4的导热性薄片。
评价
关于各实施例与比较例，对(a)非粘附性树脂层和粘附性导热层的粘性；(b)导热性薄片的导热率，(c)导热性薄片的再加工性，(d)导热性薄片的非粘附性树脂层与粘附性导热层的层间剥离强度进行如下评价。结果如表1所示。
(a)非粘附性树脂层和粘附性导热层的粘性
作为粘性试验机，使用RHESCA公司制的粘性试验机TAC-II，在按压速度30mm/min、剥离速度120mm/min、负荷196g、按压时间5.0秒、拉伸距离5mm、探针加热至40℃、薄片台加热至40℃的条件下将直径10mm的铝制圆柱状探针按压至实施例1至7及比较例1至3的导热性薄片的非粘附性树脂层并剥离时，测定探针粘附力。现在，由于在比较例4的导热性薄片中没有非粘附性树脂层，因而测定出粘附性导热层的粘性。
(b)导热性薄片的导热率
导热性薄片在厚度方向上的导热率根据ASTM D-5470标准的导热率仪(索尼制)测定(加热器输出8W、薄片表面压力1kgf/cm2)。
(c)导热性薄片的再加工性
将导热性薄片以非粘附性树脂层为下侧的方式夹置在上下平行的彼此面对的铜棒之间，在压力1kgf/cm2下放置10分钟，之后剥离棒。此时，在导热性薄片的非粘附性树脂层与铜板之间产生剥离的情况下评价为O，否则评价为×。
(d)导热性薄片的非粘附性树脂层与粘附性导热层的T型剥离强度
使用拉伸试验机(RTG-1225，Orientec社)，如图1中所示，在PET膜1层叠至非粘附性树脂层2、覆盖膜4层叠至粘附性导热层3的状态下通过T型剥离试验测定非粘附性树脂层2与粘附性导热层3的层间剥离强度。在该情况下，拉伸强度为500mm/min、样品宽度为2cm。
根据表1可知，在形成非粘附性树脂层的树脂的玻璃化转变温度为60至110℃的实施例1、2、4至7中，即使不配合固化剂，非粘附性树脂层的粘附力值仍然为6至25kN/m2，并且非粘附性树脂层与粘附性导热层的层间玻璃强度(T型剥离强度)为0.2N/cm以上，再加工性良好。
此外可知，非粘附性树脂层的厚度为20μm以下，导热性薄片具有充分的导热性。
另一方面，在非粘附性树脂层的粘附力值超过30kN/m2的比较例1、2以及无非粘附性树脂层的比较例4中，由于被粘物粘贴导热性薄片，因而再加工性劣化。此外，在非粘附性树脂层与粘附性导热层的根据T型剥离试验的层间剥离强度不到0.2N/cm的比较例3中，由于非粘附性树脂层容易从粘附性导热层剥离，因而加工性低劣。
产业上的应用可能性
根据本发明的导热性薄片，由于层叠有粘附性导热层以及比该粘附性导热层的粘性低且具有特定大小的粘性的非粘附性树脂层，因此，提高了使用导热性薄片组装电子部件和散热器时的加工性，并且也提高了对组装物体重新组装的再加工性。
虽然参照特定的实施方式对本发明进行了详细地说明，但是对本领域技术人员而言能够在不脱离本发明的精神和范围的情况下对本发明进行各种变更和修改。
本发明基于2013年3月28日申请的日本专利申请(申请号JP 2013-068724)，其内容作为参考引入本文中。
符号说明
1 PET膜
2 非粘附性树脂层
3 粘附性导热层
4 覆盖膜(PET)

Claims (7)

1.一种导热性薄片，为层叠粘附性导热层和非粘附性树脂层的导热性薄片，其特征在于，
粘附性导热层含有丙烯酸类化合物固化后的丙烯酸类树脂以及导热性填料，该丙烯酸类树脂的玻璃化转变温度为-80至15℃，粘附性导热层的粘性高于非粘附性树脂层的粘性，非粘附性树脂层的粘性为6至30kN/m2，
非粘附性树脂层的玻璃化转变温度为60至110℃，
导热性薄片在厚度方向上的导热率为1.5W/m·K以上，
其中，粘性为在按压速度30mm/min、剥离速度120mm/min、负荷196g、按压时间5.0秒、拉伸距离5mm、探针加热至40℃、薄片台加热至40℃的条件下将铝制圆柱状探针按压至该粘附性导热层或该非粘附性树脂层并剥离而作为探针粘附力进行测定的粘性。
2.一种导热性薄片，为层叠粘附性导热层和非粘附性树脂层的导热性薄片，其特征在于，
粘附性导热层含有丙烯酸类化合物固化后的丙烯酸类树脂以及导热性填料，该丙烯酸类树脂的玻璃化转变温度为-80至15℃之间，粘附性导热层的粘性高于非粘附性树脂层的粘性，
非粘附性树脂层的玻璃化转变温度为60至110℃，
非粘附性树脂层与粘附性导热层的T型剥离强度为0.2N/cm以上，
导热性薄片在厚度方向上的导热率为1.5W/m·K以上，
其中，粘性为在按压速度30mm/min、剥离速度120mm/min、负荷196g、按压时间5.0秒、拉伸距离5mm、探针加热至40℃、薄片台加热至40℃的条件下将铝制圆柱状探针按压至该粘附性导热层或该非粘附性树脂层并剥离而作为探针粘附力进行测定的粘性。
3.根据权利要求1或2所述的导热性薄片，其特征在于，形成非粘附性树脂层的树脂选自聚乙烯醇缩丁醛树脂、聚酯树脂和聚氨酯树脂中。
4.根据权利要求1或2所述的导热性薄片，其特征在于，形成粘附性导热层的丙烯酸类化合物为单官能(甲基)丙烯酸酯单体。
5.根据权利要求3所述的导热性薄片，其特征在于，形成粘附性导热层的丙烯酸类化合物为单官能(甲基)丙烯酸酯单体。
6.根据权利要求1或2所述的导热性薄片，其特征在于，相对于丙烯酸类化合物的单体单元100质量份，粘附性导热层含有选自己二酸类、癸二酸类、磷酸类、蓖麻油类、油酸类以及丙烯酸类中的一种以上增塑剂20至80质量份。
7.根据权利要求3所述的导热性薄片，其特征在于，相对于丙烯酸类化合物的单体单元100质量份，粘附性导热层含有选自己二酸类、癸二酸类、磷酸类、蓖麻油类、油酸类以及丙烯酸类中的一种以上增塑剂20至80质量份。
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