CN106459718B - 导热性导电性粘接剂组合物 - Google Patents

导热性导电性粘接剂组合物 Download PDF

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Publication number
CN106459718B
CN106459718B CN201580028049.0A CN201580028049A CN106459718B CN 106459718 B CN106459718 B CN 106459718B CN 201580028049 A CN201580028049 A CN 201580028049A CN 106459718 B CN106459718 B CN 106459718B
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adhesive composition
electrically conductive
thermally
conductive adhesive
acid
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CN106459718A (zh
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阿部真太郎
古正力亚
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Tanaka Kikinzoku Kogyo KK
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Tanaka Kikinzoku Kogyo KK
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    • C09J9/02—Electrically-conducting adhesives
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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Abstract

本发明涉及一种导热性导电性粘接剂组合物，其包含(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂，其中：所述(A)导电性填料为具有1至10μm的平均粒径的银粉，所述(B)环氧树脂在1分子内具有2个以上的环氧官能团及芳香环，所述(C)反应性稀释剂为在脂肪族烃链中具有2个以上的缩水甘油醚官能团且分子量为150至600的化合物，并且所述(D)固化剂为在1分子内具有2个以上的酚官能团的化合物、在1分子内具有2个以上的苯胺官能团的化合物、或这些化合物的混合物，所述(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂的含量分别在特定范围内。本发明的导热性导电性粘接剂组合物具有高导热性与稳定的导电性。

Description

导热性导电性粘接剂组合物
技术领域
本发明涉及一种导热性导电性粘接剂组合物。
背景技术
近年来，对于小型化、高功能化的电子零件(例如功率器件或发光二极管(LED))的需求急速扩大。功率器件作为可抑制电力损耗并高效率地转换电力的半导体元件，在电动汽车、混合动力汽车、快速充电器等领域中普及发展，此外在太阳能发电系统、百万瓦级太阳能系统等新能源领域中，其需求的提高也备受期待。
另一方面，相较于白炽灯泡具有长寿命、小型、低消耗电力等优点的LED元件在照明、便携电话、液晶面板、汽车、信号机、街灯、影像显示装置等各种领域中快速地普及。
在如上所述的电子零件的小型化、高功能化的进展中，半导体元件的发热量具有增大的倾向。然而，若电子零件长时间暴露在高温环境下，则变得无法发挥原本的功能或寿命减少。因此，为了使从半导体元件产生的热有效地扩散，在用于芯片接合的接合材料(芯片接合材料)中，通常使用高散热性的接合材料。虽也因用途而异，但接合材料通常必须具有将从半导体元件产生的热有效率地散往基板、壳体的功能，即要求有高散热性。
如此，用于电子零件的接合材料由于要求具有高散热性，因此常规上广泛使用含有大量铅的高温铅焊料或含有大量金的金锡焊料。然而，高温铅焊料具有含有对人体有害的铅的问题。因此，无铅化的技术开发最近变得活跃，关于切换至无铅焊料的研究正积极发展。另一方面，金锡焊料含有昂贵的金，故具有成本方面的问题。
在这样的情况下，近年来，作为替代高温铅焊料或金锡焊料的有力代替材料，各向同性导电性粘接剂(以下简记为“导电性粘接剂”)备受瞩目。导电性粘接剂为具有导电性等功能的金属粒子(例如银、镍、铜、铝、金)与具有粘接功能的有机粘接剂(例如环氧树脂、硅树脂、丙烯酸树脂、氨基甲酸酯树脂)的复合体，其使用多样的金属粒子及有机粘接剂。由于导电性粘接剂在室温下为液体因而使用便利性良好、无铅且成本低，因此其为高温铅焊料或金锡焊料的有力替代材料，预测其市场将大幅扩大。
如上所述，作为焊料的替代材料的导电性粘接剂要求为兼具导电性和高散热性。对于作为导电性粘接剂原料的有机粘接剂，其热传导率基本上低于金属，因而通过掺合导热性的填料来赋予散热性的功能。如何减少导电性粘接剂的热阻，使产生的热有效地散逸，成为导电性粘接剂的技术开发的焦点。
常规上，关于将导热性提高的导电性粘接剂，(例如)在专利文献1中提出了一种高导热性导电性组合物，其中作为组合物中的固体成分，至少包含5至80重量％的平均纤维直径为0.1至30μm、长径比为2至100、平均纤维长度为0.2至200μm、真密度为2.0至2.5g/cc的沥青系石墨化碳纤维填料、15至90重量％的平均粒径为0.001至30μm的金属微粒填料、以及5至50重量％的粘结剂树脂。
此外，专利文献2提出了一种导电性组合物，其含有环氧树脂作为基材树脂，含有酚系固化剂作为固化剂，含有氨基甲酸酯改性环氧树脂作为柔韧性赋予剂，进一步含有金、银、铜、铁、铝、氮化铝、氧化铝、结晶二氧化硅等粉末作为导热性填充剂。
此外，在专利文献3中提出了一种粘接剂，其包含树脂成分、高导热性纤维状填料、以及由选自由银、金、铂、氮化铝、氧化硅、氧化铝及炭黑所组成的组中的至少一种所构成的高导热性球状填料，其中相对于100体积份的所述树脂成分，含有0.1至20体积份的所述高导热性纤维状填料以及10至200体积份的所述高导热性球状填料。
现有技术文献
专利文献1：日本特开2008-186590号公报
专利文献2：日本特开平6-322350号公报
专利文献3：日本特开2009-84510号公报
发明内容
发明所要解决的课题
如上所述，在电子零件的小型化、高功能化的发展中，以谋求适当的散热对策为必要的课题，兼具散热性与导电性的导电性粘接剂的开发备受期待。于是，本发明的目的在于提供一种导热性导电性粘接剂组合物，其作为芯片接合材料使用，并且具有高导热性及稳定的导电性。
解决课题的手段
本申请发明人为了达成上述目的而进行研究，结果发现在构成导电性粘接剂组合物的成分当中，通过特别限定作为导电性填料的银粉的平均粒径及其含量，同时掺合特定量的特定环氧树脂、反应性稀释剂及固化剂，即可解决上述课题，进而完成本发明。
即，本发明如下所述。
1.一种导热性导电性粘接剂组合物，其包含(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂，其中：
所述(A)导电性填料为具有1至10μm的平均粒径的银粉，并且相对于所述导热性导电性粘接剂组合物的总量，所述(A)导电性填料的含量为85至94质量％的范围；
所述(B)环氧树脂在1分子内具有2个以上的环氧官能团及芳香环，并且相对于所述导热性导电性粘接剂组合物的总量，所述(B)环氧树脂的含量为1至8质量％的范围；
所述(C)反应性稀释剂为在脂肪族烃链中具有2个以上的缩水甘油醚官能团且分子量为150至600的化合物，并且相对于所述导热性导电性粘接剂组合物的总量，所述(C)反应性稀释剂的含量为0.2至5质量％的范围；并且
所述(D)固化剂为在1分子内具有2个以上的酚官能团的化合物、在1分子内具有2个以上的苯胺官能团的化合物、或这些化合物的混合物，并且相对于所述导热性导电性粘接剂组合物的总量，所述(D)固化剂的含量为0.2至3质量％的范围。
2.如1所述的导热性导电性粘接剂组合物，其中进一步包含未表现出与所述(D)固化剂的反应性的(E)橡胶系树脂，其中相对于所述导热性导电性粘接剂组合物的总量，该(E)橡胶系树脂的含量为0.2至2质量％的范围。
3.如1所述的导热性导电性粘接剂组合物，其中对于将所述导热性导电性粘接剂组合物中的所述(A)导电性填料去除的组合物，其由以下测定值所算出的TI值(触变指数)为1至3，该测定值为利用旋转式粘度计在0.5rpm及5rpm的转速下测定的值。
本发明的效果
根据本发明，可低价地提供一种具有高散热性与稳定导电性的导热性导电性粘接剂组合物。
具体实施方式
本发明的导热性导电性粘接剂组合物(以下简记为“粘接剂组合物”)包含上述(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂作为必要成分。本发明的粘接剂组合物中，促进了(A)导电性填料的颈缩(ネッキング)，在加热固化中使分散的导电性填料彼此融合，从而充分地形成输送热的导电性填料的网络，由此呈现高散热性。
需要说明的是，本发明所使用的(A)导电性填料为具有1至10μm的平均粒径的银粉，这种微米级的银粉相较于亚微米级以下的银粉，在银粉间或银粉内的空隙较多，不仅表面容易被氧化，表面活性也较低，故常规上被认为无法形成颈缩。若可以使用微米级的银粉，则可得到颈缩所带来的高导电性及导热性，此外，相较于亚微米级以下的银粉，粘接剂固化后的收缩会受到抑制，因此在可得到与被粘接材料具有高密合性的观点上变得特别有利。此外，这种微米级的银粉的振实密度优选为4至8g/cm3。振实密度通过(例如)JIS规格Z2512:2012的金属粉-振实密度测定方法进行测定而算出。
于是本申请发明人进行深入研究，结果发现，微米级银粉形成颈缩的理由虽然尚不明确，但通过并用特定量的特定(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂而成为可能。这种见解在常规技术中尚为未知。
以下将针对(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂的各成分进行详细说明。
(A)导电性填料使用微米级，即具有1至10μm的平均粒径的银粉。若银粉的平均粒径超过10μm，则银粉间或银粉内的空隙较大，即使进行颈缩，也难以得到高导电性，故不优选。若银粉的平均粒径小于1μm，则会变得无法抑制粘接剂固化后的收缩，故会降低与被粘接材料的密合性。银粉的平均粒径更优选为1.5μm至8μm。此外，银粉的平均粒径指的是通过激光衍射法所测定的值。
在本发明中，(A)导电性填料的银粉的平均粒径为使用激光衍射·散射式粒度分析计所测定的粒径分布的50％平均粒径(D50)。例如，可使用日机装株式会社制的激光衍射·散射式粒度分析计MT-3000进行测定。
该银粉的形状并没有特别限定，可列举出球状、片状、箔状、树枝状等，但一般选择片状或球状。此外，对于银粉，除了纯银粉以外，也可使用被银被覆表面的金属粒子、或者这些的混合物。银粉可由市售品取得，或可用公知的方法进行制作。制作银粉的方法并没有特别限制，可任意使用机械性粉碎法、还原法、电解法、气相法等。
(A)导电性填料的银粉的表面可以被涂布剂被覆。可列举出(例如)含羧酸的涂布剂。通过使用含羧酸的涂布剂，可进一步提高粘接剂组合物的散热性。
该涂布剂所包含的羧酸并没有特别限定，可列举出：单羧酸、多羧酸、氧羧酸等。
作为所述单羧酸，可列举出(例如)乙酸、丙酸、丁酸、戊酸、辛酸、己酸、癸酸、月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、花生酸、山萮酸、木蜡酸等碳原子数为1至24的脂肪族单羧酸。此外，也可使用油酸、亚油酸、α-亚麻酸、γ-亚麻酸、双高-γ-亚麻酸、反油酸、花生四烯酸、芥酸、神经酸、十八碳四烯酸、二十碳五烯酸、二十二碳六烯酸等碳原子数为4至24的不饱和脂肪族羧酸。再者，也可使用苯甲酸、萘甲酸等碳原子数为7至12的芳香族单羧酸等。
作为所述多羧酸，可列举出(例如)乙二酸、丙二酸、琥珀酸、戊二酸、己二酸、壬二酸、癸二酸等碳原子数为2至10的脂肪族多羧酸；马来酸、富马酸、衣康酸、山梨酸、四氢邻苯二甲酸等碳原子数为4至14的脂肪族不饱和多羧酸；邻苯二甲酸、偏苯三甲酸等芳香族多羧酸等。
作为所述氧羧酸，可列举出(例如)乙醇酸、乳酸、氧丁酸、甘油酸等脂肪族羟基单羧酸；水杨酸、氧苯甲酸、没食子酸等芳香族羟基单羧酸；酒石酸、柠檬酸、苹果酸等羟基多羧酸等。
为了降低银粉的凝聚，用以处理该银粉表面的涂布剂中可包含碳原子数为10以上的高级脂肪酸或其衍生物。这种高级脂肪酸可列举出(例如)月桂酸、肉豆蔻酸、棕榈酸、硬脂酸、油酸、亚油酸、亚麻酸、木蜡酸。高级脂肪酸的衍生物可列举出(例如)高级脂肪酸金属盐、高级脂肪酸酯、高级脂肪酸酰胺。
该涂布剂所包含的羧酸也可为2种以上的前述羧酸的混合物。此外，上述羧酸当中，优选碳原子数为12至24的饱和脂肪酸或不饱和脂肪酸的高级脂肪酸。
采用涂布剂被覆该银粉表面时，可以利用以下公知的方法：在混合器中搅拌并捏合两者的方法、将该银粉浸入羧酸的溶液后使溶剂挥发的方法等。
在本发明的粘接剂组合物中，在不损及本发明的效果的范围内，可并用其他导电性填料。作为这种导电性填料，只要是具有导电性的物质，则没有特别的限定，但优选金属或纳米碳管。作为金属，可作为一般导体处理的金属粉末皆可使用。可列举出(例如)镍、铜、银、金、铝、铬、铂、钯、钨、钼等的单体、由这些2种以上的金属构成的合金、这些金属的涂布制品、或者为这些金属的化合物且具有良好导电性的物质等。
相对于粘接剂组合物的总量，可含有85至94质量％范围的(A)导电性填料。若(A)导电性填料的含量小于85质量％，则会变得难以抑制颈缩率的降低或粘接剂固化后的收缩，造成导热性或导电性降低，与被粘接材料的密合性也变差；反之，若超过94质量％，则难以变成膏状，与被粘接材料的充分的密合性也变差。(A)导电性填料的优选的含量为88至94质量％，更优选的含量为89至93质量％。
(B)环氧树脂为在1分子内具有2个以上的环氧官能团及芳香环的化合物，本发明使用液状的环氧树脂。可仅使用一种，也可并用两种以上。这种液状的环氧树脂的具体例子可为表氯醇与双酚类等多元酚类或多元醇进行缩合后所得的环氧树脂，可列举出(例如)双酚A型、溴化双酚A型、氢化双酚A型、双酚F型、双酚S型、双酚AF型、联苯型、萘型、芴型、酚醛清漆型、苯酚酚醛清漆型、邻甲酚酚醛清漆型、三(羟苯基)甲烷型、四羟苯基乙烷型等的缩水甘油醚型环氧树脂。此外，可列举出表氯醇与邻苯二甲酸衍生物或脂肪酸等羧酸进行缩合所得的缩水甘油酯型环氧树脂，进一步可列举出以各种方法所改性的环氧树脂，但并不限定于此。特别优选使用双酚型环氧树脂，其中优选使用双酚A型、双酚F型的环氧树脂。
相对于粘接剂组合物的总量，含有1至8质量％范围的(B)环氧树脂。若(B)环氧树脂的含量小于1质量％，则粘接力会变弱，连接可靠性会降低。反之，若超过8％质量，则变得难以通过导电性填料的颈缩而形成网络，从而无法得到稳定的导电性、导热性。(B)环氧树脂的优选含量为1.4至3.5质量％。
(C)反应性稀释剂为脂肪族烃链中具有2个以上的缩水甘油醚官能团且分子量为150至600的化合物。此外，除了缩水甘油醚官能团以外，也可具有其他聚合性官能团，例如乙烯基、烯丙基等的烯基；丙烯酰基、甲基丙烯酰基等的不饱和基团。若分子量小于150，则在进行固化反应之前，反应性稀释剂便会挥发从而无法得到预定的粘接特性；反之，若超过600，则反应性稀释剂的反应性会变慢，从而难以得到预期的效果。更加优选的分子量为200至500。
这种反应性稀释剂可列举出(例如)乙二醇二缩水甘油醚、丙二醇二缩水甘油醚、丁二醇二缩水甘油醚、新戊二醇二缩水甘油醚、环己烷二甲醇二缩水甘油醚之类的二环氧化物；苯基缩水甘油醚、丁基苯基缩水甘油醚之类的单环氧化物；三羟甲基丙烷三缩水甘油醚、甘油三缩水甘油醚之类的三环氧化物等。
其中，从提高本发明的效果的观点来看，优选为丁二醇二缩水甘油醚、环己烷二甲醇二缩水甘油醚、丁基苯基缩水甘油醚等。
相对于粘接剂组合物的总量，含有0.2至5质量％范围的(C)反应性稀释剂。若(C)反应性稀释剂的含量小于0.2质量％，则树脂成分会难以分散从而变得不均匀，与被粘接材料的密合性便会降低。反之，若超过5质量％，则固化后的树脂会变脆，与被粘接材料的密合性降低，且恐怕会因断裂等导致导电性降低。(C)反应性稀释剂的优选含量为0.3至1.2质量％。
(D)固化剂为1分子内具有2个以上的酚官能团的化合物、1分子内具有2个以上的苯胺官能团的化合物、或者这些化合物的混合物。
1分子内具有2个以上的酚官能团的化合物可列举出(例如)如下的化合物。
[化1]
Figure BDA0001163419470000081
式中，R1至R5各自独立地表示碳原子数为1至5的烷基、烯丙基或氢原子。n表示0以上的整数。
可使用市售品作为这种1分子内具有2个以上的酚官能团的化合物，例如，可列举出明和化成株式会社制的MEH8000系列(8000H、8005、8010、8015)等。其中，从提高本发明的效果的观点来看，优选MEH8000H(上式中，R1至R5为氢或烯丙基、n为0至3的化合物)。
此外，1分子内具有2个以上的苯胺官能团的固化剂可列举出如下通式(I)、(II)或(III)所表示的化合物作为优选的例子。下列通式(I)、(II)或(III)所表示的化合物也可根据需要组合2种以上。此外，本发明所提及的低级烷基，可列举出碳原子数为1至6的直链、分枝或环状的烷基，优选为碳原子数为1至3的直链或分枝的烷基，特别优选为甲基或乙基。
特别是下列通式(I)、(II)或(III)所表示的化合物的群当中式中X为-SO2-的二氨基二苯砜及其衍生物可得到适当的固化延迟效果，此外，可促进由与导电性填料的相互作用所带来的导电性填料的烧结成长及网络形成，故优选使用；4,4’-二氨基二苯砜及3,3’-二氨基二苯砜的前述效果最强，最适合使用。此外，在不损及本发明的效果下，也可并用其他公知的固化剂。
[化2]
Figure BDA0001163419470000091
式中，X表示-SO2-、-CH2-或-O-，R1至R4各自独立地表示氢原子或低级烷基。
[化3]
Figure BDA0001163419470000092
式中，X表示-SO2-、-CH2-或-O-，R5至R8各自独立地表示氢原子或低级烷基。
[化4]
Figure BDA0001163419470000101
式中，X表示-SO2-、-CH2-或-O-，R9至R12各自独立地表示氢原子或低级烷基。
相对于粘接剂组合物的总量，含有0.2至3质量％范围的(D)固化剂。若(D)固化剂的含量小于0.2质量％，则会有因固化不充分而耐热性差的情况。此外，即使在固化充分的情况下，树脂的固化速度与由导电性填料的烧结颈缩而导致的网络形成速度也无法适当平衡，导电性或导热性恐怕会降低。反之，若超过3质量％，则由于未反应的固化剂残留而与被粘接材料的密合性降低，故不仅电特性降低，树脂的固化速度与由导电性填料的烧结颈缩而导致的网络形成速度也无法适当平衡，导电性或导热性恐怕会降低。(D)固化剂的优选的含量为0.2至2.5质量％，更优选的含量为0.3至2质量％。
本发明中，优选进一步含有未表现出与固化剂的反应性的(E)橡胶系树脂，其中相对于所述粘接剂组合物的总量，所述(E)橡胶系树脂的含量为0.2至2质量％。通过掺合该(E)橡胶系树脂，可进一步促进(A)导电性填料的颈缩，从而能呈现高散热性。
作为(E)橡胶系树脂，可列举出(例如)酸改性橡胶。其中，优选室温下为液状的液状橡胶系树脂，更优选具有羧基的液状丙烯腈丁二烯橡胶。作为具有羧基的丙烯腈丁二烯橡胶，可列举出下式所表示的化合物。
[化5]
Figure BDA0001163419470000102
式中，m表示5至50的整数，a和b各自独立地表示1以上的整数。a与b的比(a/b)优选为95/5至50/50。这种化合物(例如)可由市售品的Hycar CTBN-2009×162、CTBN-1300×31、CTBN-1300×8、CTBN-1300×13、CTBN-1009SP-S、CTBNX-1300×9、ATBN-1300×16、ATBN-1300×21、ATBN-1300×35、ATBN-1300×42、ATBN-1300×45(任一均为宇部興産株式会社制)取得。优选使用CTBN系列。
相对于粘接剂组合物的总量，(E)液状橡胶系树脂的含量优选为0.2至2质量％，更优选为0.2至1.5质量％，最优选为0.4至1.1质量％。
关于本发明的粘接剂组合物，在热固化时的(A)导电性填料开始烧结之前，要求该组合物为未固化或半固化的状态。若在热固化时的(A)导电性填料开始烧结之前，粘接剂组合物为完全固化的状态，则变得无法得到良好的导热性。
此处，所谓的在热固化时的(A)导电性填料开始烧结之前，指的是在使粘接剂组合物热固化时开始加热之后，(A)导电性填料烧结、平均粒径成长之前的状态。此外，粘接剂组合物为未固化的状态，指的是在可溶解该粘接剂组合物的溶剂(四氢呋喃)中，实质上完全溶解的状态。此外，粘接剂组合物为半固化的状态，指的是该粘接剂组合物的固化在中间阶段，可以说是处于可进行进一步固化的状态。半固化的状态为一部分溶解于可溶解粘接剂组合物的溶剂(四氢呋喃)中的状态。
在本发明中，在热固化时的(A)导电性填料开始烧结之后，该导电性填料的平均粒径成长率达到30％时的粘接剂组合物的固化率特别优选为50％以下。若固化率高于50％，则恐怕会无法得到高导热性。
在本发明中，颈缩指的是粘接剂组合物的固化体中的导电性填料彼此之间不单单只有接触，更有一部分因烧结而处于接续连接的状态，颈缩率为在200℃下进行1小时的热处理后，对粘接剂组合物的固化体的垂直剖面进行SEM图像观察，由此评价其颈缩的粒子的比例的值。具体而言，为观察剖面图像大约中心部分30×30μm正方形的图像，并用与各导电性填料粒子连接的粒子数(1+连接粒子数)的和除以导电性填料粒子数而得的数值(下式)。例如，在观察图像中具有100个电性填料粒子，且各粒子连接的粒子数全部为2的情况下，与各导电性填料粒子连接的粒子的总和为300。此情况下，颈缩率为300％。
[式]颈缩率(％)＝100ד1+与各导电性填料粒子连接的粒子的总和”÷“导电性填料粒子数”
本发明中，可通过使用环氧固化剂来任意地调节粘接剂组合物的固化率。环氧固化剂可列举出(例如)甲阶段型酚醛树脂(レゾール型フェノール樹脂)、酚醛清漆型酚醛树脂(ノボラック型フェノール樹脂)、酸酐类、叔胺类、三苯基膦类等的固化催化剂；二氰二酰胺类、肼类、芳香族二胺类等的阴离子聚合型固化剂；有机过氧化物等，但特别优选使用甲阶段型酚醛树脂。甲阶段型酚醛树脂为由酚类与醛类的反应所产生的树脂，其羟基具有与环氧基进行反应而使环氧树脂的分子链交联化而固化的功能。环氧固化剂可仅使用一种，也可并用两种以上。
甲阶段型酚醛树脂的掺合量并没有限定，根据环氧树脂的种类或量等而适当决定即可，但使用时相对于本发明的粘接剂组合物的总量，一般为0.1至4质量％。
本发明的粘接剂组合物中也可掺合固化促进剂。固化促进剂可列举出(例如)2-苯基-4,5-二羟甲基咪唑、2-苯基-4-甲基-5-羟甲基咪唑、2-甲基-4-甲基咪唑、1-氰基-2-乙基-4-甲基咪唑等的咪唑类、叔胺类、三苯膦类、尿素系化合物、酚类、醇类、羧酸类等。固化促进剂可仅使用一种，也可并用两种以上。
固化促进剂的掺合量并没有限定，只要适当决定即可，但使用时，相对于本发明的粘接剂组合物的总量，一般为0.1至2质量％。
本发明的粘接剂组合物中也可掺合溶剂。溶剂可列举出(例如)丁基卡必醇、丁基卡必醇乙酸酯、乙基卡必醇、乙基卡必醇乙酸酯、丁基溶纤剂、丁基溶纤剂乙酸酯、乙基溶纤剂、乙基溶纤剂乙酸酯、γ-丁内酯、异佛尔酮、缩水甘油基苯基醚、三乙二醇二甲醚等的有机溶剂。溶剂可仅使用一种，也可并用两种以上。
溶剂的掺合量并没有限定，只要适当决定即可，使用时相对于本发明的粘接剂组合物的总量，一般为0.1至5.0质量％。
本发明的粘接剂组合物中，在不损及本发明的效果的范围内，也可适当掺合抗氧化剂、紫外线吸收剂、增粘剂、分散剂、偶联剂、韧性赋予剂、弹性体等作为其他添加剂。
本发明的粘接剂组合物可通过以任意的顺序混合、搅拌上述(A)成分、(B)成分、(C)成分、(D)成分以及根据需求而加入的(E)成分与其他成分而得到。分散的方法可采用二辊磨、三辊磨、砂磨机、辊磨机、球磨机、胶体磨机、喷射磨机、珠磨机、捏合机、均质机、无螺旋桨式混合机等的方式。
需要说明的是，对于本发明的粘接剂组合物，在使用(E)成分的情况下，通过事先混合(A)成分及(E)成分，之后再混合其他各种成分并进行搅拌，理由虽尚不明确，但由此可进一步促进(A)导电性填料的颈缩，从而可得到高导热性并表现散热性。
在去除如上述所调制的粘接剂组合物中的(A)导电性填料的情况下的粘度通过旋转式粘度计进行测定。此外，在本发明中，上述粘度为使用锥板型粘度计作为旋转式粘度计，在25℃的温度下使用3°×R14锥板，并以特定的转速(rpm)所测定的值。
此外，对于如上述所调制的粘接剂组合物，在去除其中的(A)导电性填料的情况下，由利用旋转式粘度计在转速0.5rpm及5rpm下测定的值所算出TI值(触变指数)优选为1至3。通过具有该TI值，不仅可提高制作浆料时的操作性，更可发挥以下效果：使电性填料与树脂适当地分散，并促进热固化时的导电性填料的颈缩化，进而可得到更高导热性与导电性。此外，在本发明中，上述TI值为用上述旋转式粘度计在0.5ppm的转速下的测定值除以在5ppm的转速下的测定值而算出的值。
实施例
以下，通过实施例进一步具体说明本发明，但本发明并不受这些实施例的任何限制。
[实施例1至9、比较例1至3]
A.粘接剂组合物的制作
以三辊磨对表1所记载的各材料进行捏合，以制作表1所示的组成的粘接剂组合物(各材料的数值表示相对于粘接剂组合物的总质量的质量％)。使用的材料如下所述。此外，捏合的顺序是：先进行(A)成分及(E)成分的捏合，接着，混合其他各种成分并捏合使各成分为均匀分散的状态。在200℃下加热1小时后冷却至室温，得到粘接剂组合物的固化体。
(A)导电性填料
·银粉[平均粒径：5.0μm，田中貴金属工業(株)制]振实密度为6.5g/cm3
·银粉[平均粒径：1.5μm，田中貴金属工業(株)制]振实密度为4.7g/cm3
·银粉[平均粒径：8.0μm，田中貴金属工業(株)制]振实密度为4.2g/cm3
(B)环氧树脂
·双酚F型环氧树脂[EPICRON EXA-830CRP，DIC(株)制，室温下为液状]
·苯酚酚醛清漆型环氧树脂(jER-152，三菱化学(株)社制，室温下为液状)
·萘型环氧树脂(DIC(株)社制HP4032D，室温下为液状)
(C)反应性稀释剂
·1,4-丁二醇二缩水甘油醚(分子量为202.25)
·1,4-环己烷二甲醇二缩水甘油醚(分子量为256.34)
(D)固化剂
·1分子内具有2个以上的酚官能团的化合物[明和化成(株)制的MEH8000H]
·1分子内具有2个以上的苯胺官能团的化合物[東京化成工業(株)制的4,4’-二氨基二苯砜]
(E)液状橡胶系树脂
·具有羧基的丙烯腈丁二烯橡胶[宇部興産(株)制的CTBN-1300×13NA]
(固化促进剂)
·甲苯双二甲基脲[Carbon Scientific社制]
·咪唑系固化促进剂[四国化成工業(株)社制的2P4MHZ]
(溶剂)
·γ-丁内酯
·N-甲基吡咯烷酮
(其他)
·核壳颗粒[アイカ工業(株)制的AC-3355]
·硅烷偶联剂(東レ·ダウコーニング(株)社制的Z-6040)
B.粘接剂组合物的物性评价
1.粘度
调制将(A)导电性填料去除的粘接剂组合物，并测定其粘度。粘度为使用锥板型粘度计作为旋转式粘度计，在25℃的温度下使用3°×R14锥板，并以0.5ppm或5ppm的转速在25℃的温度下进行测定。结果显示于表1。
2.TI值
调制将(A)导电性填料去除的粘接剂组合物，并测定其TI值。TI值为用上述旋转式粘度计在0.5ppm的转速下的测定值除以在5ppm的转速下的测定值而算出。结果显示于表1。
3.热传导率的测定
为了评价该粘接剂组合物的热传导特性，测定该粘接剂组合物的热传导率。使用激光闪光法热常数测定装置(TC-7000、ULVAC-RIKO社制)，根据ASTM-E1461测定热扩散a，通过比重计方法算出室温下的比重d，使用差示扫描量热测定装置(DSC7020，セイコー電子工業社制)，根据JIS-K7123测定室温下的比热Cp，并以下式算出热传导率λ(W/m·K)。结果显示于表1。
λ＝a×d×Cp
4.体积电阻率的测定
为了评价该粘接剂组合物的电特性，测定该粘接剂组合物的体积电阻率。使用直流电压·发生源监视器(R6243，ADVANTEST社制)，通过直流4端子法来测定表观电阻R，由测定样本的宽度W、厚度T及长度L，以下式计算得出体积电阻率K(×10-4Ω·cm)。结果显示于表1。
K＝L/(R×W×T)
5.颈缩率的测定
以分配器将粘接剂组合物涂布于2×2mm的正方形的镀银的铜制基板上后，以硅制的2×2mm的正方形的基板与铜板夹住粘接剂组合物的形态进行装载放置，并在200℃下热处理1小时后，对粘接剂组合物的固化体的垂直剖面进行SEM图像观察，由此评价颈缩率。具体而言，对于粘接剂组合物的固化体的剖面图像大约中心部位的任意5处，分别观察30×30μm的正方形的图像，并由用与各导电性填充粒子连接的粒子数(1+连接粒子数)的和除以导电性填料粒子数的数值(下式)的平均值从而算出颈缩率。算出结果显示于表1。
[式]颈缩率(％)＝100ד1+与各导电性填料粒子连接的粒子的总和”÷“导电性填料粒子数”
Figure BDA0001163419470000171
由上述结果可确认，本发明的粘接剂组合物具有高热传导率与稳定的导电性。
虽参照特定的方案详细说明了本发明，但对于本领域技术人员显而易见的是，可以在不脱离本发明的精神和范围内进行各种变更及修正。
需要说明的是，本申请基于2014年5月29日所申请的日本专利申请(特愿2014-111769)，将其全文内容引用至本文。

Claims (2)

1.一种导热性导电性粘接剂组合物，其包含(A)导电性填料、(B)环氧树脂、(C)反应性稀释剂以及(D)固化剂，其中，
所述(A)导电性填料为具有1至10μm的平均粒径的银粉，所述银粉的表面被含羧酸的涂布剂被覆，并且相对于所述导热性导电性粘接剂组合物的总量，所述(A)导电性填料的含量为85至94质量％的范围；
所述(B)环氧树脂在1分子内具有2个以上的环氧官能团及芳香环，并且相对于所述导热性导电性粘接剂组合物的总量，所述(B)环氧树脂的含量为1至8质量％的范围；
所述(C)反应性稀释剂为在脂肪族烃链中具有2个以上的缩水甘油醚官能团且分子量为150至600的化合物，并且相对于所述导热性导电性粘接剂组合物的总量，所述(C)反应性稀释剂的含量为0.2至5质量％的范围；并且
所述(D)固化剂为在1分子内具有2个以上的酚官能团的化合物、在1分子内具有2个以上的苯胺官能团的化合物、或这些化合物的混合物，并且相对于所述导热性导电性粘接剂组合物的总量，所述(D)固化剂的含量为0.2质量％以上且小于2质量％的范围，
进一步包含未表现出与所述(D)固化剂的反应性的(E)橡胶系树脂，其中相对于所述导热性导电性粘接剂组合物的总量，所述(E)橡胶系树脂的含量为0.2至2质量％的范围。
2.根据权利要求1所述的导热性导电性粘接剂组合物，其中对于将所述导热性导电性粘接剂组合物中的所述(A)导电性填料去除的组合物，其由以下测定值所算出的TI值(触变指数)为1至3，该测定值为利用旋转式粘度计在0.5rpm及5rpm的转速下测定的值。
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