TWI554588B - A thermally conductive conductive agent composition - Google Patents

A thermally conductive conductive agent composition Download PDF

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Publication number
TWI554588B
TWI554588B TW104117356A TW104117356A TWI554588B TW I554588 B TWI554588 B TW I554588B TW 104117356 A TW104117356 A TW 104117356A TW 104117356 A TW104117356 A TW 104117356A TW I554588 B TWI554588 B TW I554588B
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Taiwan
Prior art keywords
conductive
adhesive composition
acid
mass
conductive adhesive
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TW104117356A
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English (en)
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TW201606044A (zh
Inventor
Shintaro Abe
Rikia FURUSHO
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Tanaka Precious Metal Ind
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    • C09J9/02—Electrically-conducting adhesives
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    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • 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
    • C08G59/50—Amines
    • C08G59/5033—Amines aromatic
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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
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    • C08G59/50—Amines
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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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Description

導熱性導電性接著劑組成物
本發明係關於一種導熱性導電性接著劑組成物。
近年來，小型化、高功能化的電子零件的需求急速擴大，例如功率元件或發光二極體(LED)。功率元件作為可抑制電力損耗並高效率地轉換電力的半導體元件，在電動汽車、混合動力汽車、快速充電器等領域中普及發展，此外在太陽能發電系統、百萬瓦級太陽能(Mega Solar)系統等的新能源領域中，其需求的提高亦備受期待。
另一方面，相較於白熾燈泡，具有長壽命、小型、低消耗電力之優點的LED元件，在照明、行動電話、液晶面板、汽車、信號機、街燈、影像顯示裝置等各種領域中快速地普及。
在如上述電子零件之小型化、高功能化的進展中，半導體元件的發熱量具有增大的傾向。然而，若電子零件長時間暴露於高溫環境下，則變得無法發揮原本的功能或壽命減低。因此，為了使從半導體元件產生的熱有效地擴散，用於晶粒接合的接合材料(晶粒接合材料)中，通常使用高散熱性的接合材料。雖亦因用途而異，但接合材料通常必須具有使從半導體元件產生的熱有效率地散往基板、殼體的功能，即要求高散熱性。
如此，用於電子零件的接合材料由於被要求具有高散熱性，故以往廣泛使用含有大量鉛的高溫鉛軟焊料或含有大量金的金錫焊料。然 而，高溫鉛軟焊料具有含有對人體有害之鉛的問題。因此，無鉛化的技術開發最近變得活躍，關於切換至無鉛焊料的研究正積極發展。另一方面，金錫焊料含有昂貴的金，故具有成本方面的問題。
在這樣的狀況下，近年來，作為替代高溫鉛軟焊料或金錫焊料的有力替代材料，等向性導電性接著劑(以下僅記載為「導電性接著劑」)頗受矚目。導電性接著劑係具有導電性等功能之金屬粒子(例如銀、鎳、銅、鋁、金)與具有接著功能之有機接著劑(例如環氧樹脂、矽氧樹脂、丙烯酸樹脂、胺基甲酸酯樹脂)的複合體，其使用多樣的金屬粒子及有機接著劑。由於導電性接著劑在室溫下為液體、使用性良好、無鉛且成本低，因此係高溫鉛軟焊料或金錫焊料的有力替代材料，預測其市場將大幅擴大。
如上所述，作為焊料之替代材料的導電性接著劑，係要求兼具導電性與高散熱性。導電性接著劑原料的有機接著劑，基本上熱傳導率低於金屬，故藉由摻合導熱性的填充劑來賦予散熱性的功能。如何減小導電性接著劑的熱阻，使產生的熱有效地散逸，成為導電性接著劑之技術開發的焦點。
以往，關於將導熱性提高的導電性接著劑係如在專利文獻1中所提出的高導熱性導電性組成物，其中組成物中的固體成分係至少包含一平均纖維直徑0.1~30μm、縱橫比2~100、平均纖維長度0.2~200μm、真密度2.0~2.5g/cc的瀝青系石墨化碳纖維填充劑5~80重量%、一平均粒徑0.001~30μm的金屬微粒子填充劑15~90重量%、及一黏結劑樹脂5~50重量%。
此外，專利文獻2中提出了一種導電性組成物，其含有環氧樹脂作為基材樹脂，含有酚系硬化劑作為硬化劑，含有胺基甲酸酯改質環 氧樹脂作為可撓性賦予劑，進一步含有金、銀、銅、鐵、鋁、氮化鋁、氧化鋁、晶性矽石等的粉末作為導熱性填充劑。
此外，在專利文獻3中提出了一種接著劑，其係包含樹脂成分、高導熱性纖維狀填充劑、及選自由銀、金、鉑、氮化鋁、氧化矽、氧化鋁及碳黑所組成之群組的至少1種，所構成的高導熱性球狀填充劑的接著劑，相對於該樹脂成分100體積份，含有0.1~20體積份的該高導熱性纖維狀填充劑、並含有10~200體積份的該高導熱性球狀填充劑。
【先前技術文獻】 【專利文獻】
[專利文獻1]日本特開2008-186590號公報
[專利文獻2]日本特開平6-322350號公報
[專利文獻3]日本特開2009-84510號公報
如上所述，在電子零件之小型化、高功能化的發展中，謀求適當的散熱對策係必要的課題，兼具散熱性與導電性之導電性接著劑的開發備受期待。於是，本發明之目的在於提供一種導熱性導電性接著劑組成物，作為晶粒接合材料使用，且具有高導熱性與穩定的導電性。
本案發明人為了達成上述目的而進行研究，結果發現於構成導電性接著劑組成物的成分之中，特別限定導電性填充劑之銀粉的平均粒徑及其含量，並摻合特定量的特定環氧樹脂、反應性稀釋劑及硬化劑後， 即可解決上述課題，進而完成本發明。
亦即，本發明係如下文所述。
1.一種導熱性導電性接著劑組成物，其係包含(A)導電性填充劑、(B)環氧樹脂、(C)反應性稀釋劑及(D)硬化劑，其中：該(A)導電性填充劑係具有平均粒徑1~10μm的銀粉，且相對於該導熱性導電性接著劑組成物的總量，該(A)導電性填充劑的含量為85~94質量%的範圍；該(B)環氧樹脂係1分子內具有2個以上環氧官能基及芳香環，相對於該導熱性導電性接著劑組成物的總量，該(B)環氧樹脂的含量為1~8質量%的範圍；該(C)反應性稀釋劑係於脂肪族烴鏈中具有2個以上環氧丙基醚官能基且分子量為150~600的化合物，且相對於該導熱性導電性接著劑組成物的總量，該(C)反應性稀釋劑的含量為0.2~5質量%的範圍；且該(D)硬化劑係1分子內具有2以上之酚官能基的化合物、1分子內具有2以上之苯胺官能基的化合物、或該等化合物的混合物，相對於該導熱性導電性接著劑組成物的總量，該(D)硬化劑的含量為0.2~3質量%的範圍。
2.如該1之導熱性導電性接著劑組成物，其中進一步包含未表現出與該(D)硬化劑之反應性的(E)橡膠系樹脂，且相對於該導熱性導電性接著劑組成物的總量，(E)橡膠系樹脂的含量為0.2~2質量%的範圍。
3.如該1之導熱性導電性接著劑組成物，其中將該導熱性導電性接著劑組成物中的(A)導電性填充劑去除的組成物，其由旋轉式黏度計在旋轉數0.5rpm及5rpm下之測定值所算出的TI值(搖變度)為1~3。
根據本發明，可低價地提供一種具有高散熱性與穩定導電性的導熱性導電性接著劑組成物。
本發明之導熱性導電性接著劑組成物(以下僅記載為「接著劑組成物」)，包含上述(A)導電性填充劑、(B)環氧樹脂、(C)反應性稀釋劑及(D)硬化劑作為必要成分。本發明之接著劑組成物中，促進(A)導電性填充劑的頸縮(Necking)，於加熱硬化中使分散之導電性填充劑彼此融合，而充分形成輸送熱之導電性填充劑的網絡，藉此呈現高散熱性。
此外，本發明所使用之(A)導電性填充劑，係具有平均粒徑1~10μm的銀粉，但相較於次微米級以下的銀粉，這種微米級的銀粉在銀粉間或銀粉內的空隙較多，不僅表面容易被氧化，表面活性亦較低，故以往無法形成頸縮。若可使用微米級的銀粉，則可得到頸縮所帶來的高導電性與導熱性，此外，相較於次微米級以下的銀粉，接著劑硬化後的收縮會受到抑制，故在可得到與被接著材料具有高接合性的觀點上變得特別有利。此外，這種微米級之銀粉的振實密度(tap density)為4~8g/cm3更佳。振實密度係藉由例如JIS規格Z2512：2012的金屬粉-振實密度測定方法進行測定而算出。
於是本案發明人進行深入研究，結果發現，微米級銀粉形成頸縮的理由雖然尚不明確，但可藉由併用特定量的特定(B)環氧樹脂、(C) 反應性稀釋劑及(D)硬化劑來完成。這種見解在以往技術尚為未知。
以下將針對(A)導電性填充劑、(B)環氧樹脂、(C)反應性稀釋劑及(D)硬化劑的各成分進行詳細說明。
(A)導電性填充劑中，使用微米級，亦即含有平均粒徑1-10μm的銀粉。若銀粉的平均粒徑超過10μm，則銀粉間或銀粉內的空隙較大，即使進行頸縮，亦難以得到高導電性，故不佳。若銀粉的平均粒徑小於1μm，則會變得無法抑制接著劑硬化後的收縮，故會降低與被接著材料的接合性。銀粉的平均粒徑為1.5μm~8μm更佳。此外，銀粉的平均粒徑係指藉由雷射繞射法所測定的值。
在本發明中，(A)導電性填充劑的銀粉的平均粒徑，係使用雷射繞射、散射式粒度分析計所測定之粒徑分布的50%平均粒徑(D50)。例如，可使用日機裝股份有限公司製的雷射繞射、散射式粒度分析計MT-3000進行測定。
該銀粉的形狀並無特別限定，可列舉球狀、片狀、箔狀、樹枝狀等，但一般選擇片狀或球狀。此外，銀粉除了純銀粉以外，可使用以銀被覆其表面的金屬粒子或該等的混合物。銀粉可由市售品取得，或可用習知方法進行製作。製作銀粉的方法並無特別限制，可任意使用機械性粉碎法、還原法、電解法、氣相法等。
(A)導電性填充劑的銀粉，可以塗布劑被覆其表面。可舉例如含羧酸之塗布劑。藉由使用含羧酸之塗布劑，可進一步提高接著劑組成物的散熱性。
該塗布劑所包含之羧酸並無特別限定，可列舉：單羧酸、多 羧酸、氧羧酸等。
該單羧酸可列舉如：乙酸、丙酸、丁酸、戊酸、辛酸、己酸、癸酸、月桂酸、十四酸、十六酸、硬脂酸、花生酸、萮樹酸、木蠟酸等碳數1~24的脂肪族單羧酸。此外，亦可使用十八烯酸、亞麻油酸、α-次亞麻油酸、γ-次亞麻油酸、二高-γ-亞麻油酸(dihomo-γ-linolenic acid)、反油酸、二十碳四烯酸、芥子酸、神經酸、十八碳四烯酸、二十碳五烯酸、二十二碳六烯酸等碳數4~24的不飽和脂肪族羧酸。再者，亦可使用苯甲酸、萘甲酸等碳數7~12的芳香族單羧酸等。
該多羧酸可列舉如：乙二酸、丙二酸、琥珀酸、戊二酸、己二酸、壬二酸、癸二酸等碳數2~10的脂肪族多羧酸；馬來酸、富馬酸、伊康酸、山梨酸、四氫酞酸等碳數4~14的脂肪族不飽和多羧酸；鄰苯二甲酸、偏苯三甲酸等的芳香族多羧酸等。
該氧羧酸可列舉如：乙醇酸、乳酸、氧丁酸、甘油酸等的脂肪族羥基單羧酸；水楊酸、氧苯甲酸、没食子酸等的芳香族羥基單羧酸；酒石酸、檸檬酸、蘋果酸等的羥基多羧酸等。
為了降低銀粉的凝聚，用以處理該銀粉表面的塗布劑中可包含碳數為10以上的高級脂肪酸或其衍生物。這種高級脂肪酸可例舉如月桂酸、十四酸、十六酸、硬脂酸、十八烯酸、亞麻油酸、次亞麻油酸、木蠟酸。高級脂肪酸的衍生物可例舉如：高級脂肪酸金屬鹽、高級脂肪酸酯、高級脂肪酸醯胺。
該塗布劑所包含之羧酸亦可為2種以上該羧酸的混合物。此外，上述羧酸之中，碳數12~24之飽和脂肪酸或不飽和脂肪酸的高級脂肪酸 為佳。
以塗布劑被覆該銀粉表面，只要利用「在混合器中攪拌、揉合兩者的方法」、「將該銀粉浸入羧酸的溶液後使溶劑揮發的方法」等習知的方法即可。
在本發明之接著劑組成物中，於不損及本發明之效果的範圍內，可併用其他導電性填充劑。作為這種導電性填充劑，只要是具有導電性者則並無特別限定，但金屬或奈米碳管為佳等。作為金屬，可用作一般導體處理的金屬粉末皆可使用。可列舉例如：鎳、銅、銀、金、鋁、鉻、鉑、鈀、鎢、鉬等的單體、由該等2種以上之金屬構成的合金、該等金屬的塗布製品、或該等金屬的化合物且具有良好導電性者等。
相對於接著劑組成物的總量，可含有範圍在85~94質量%的(A)導電性填充劑。若(A)導電性填充劑的含量小於85質量%，頸縮率的降低或接著劑硬化後的收縮會變得難以抑制，造成導熱性或導電性降低，與被接著材料的接合性亦變差；反之，若超過94質量%，則難以變成膏狀，與被接著材料的充分接合性亦變差。(A)導電性填充劑的含量88~94質量%為佳，含量89~93質量%為更佳。
(B)環氧樹脂係1分子內具有2個以上環氧官能基及芳香環的化合物，本發明使用液狀環氧樹脂。可僅使用一種亦可併用兩種以上。這種液狀環氧樹脂的具體例可為表氯醇與雙酚類等多元酚類或多元醇進行縮合後所得的環氧樹脂，例如，可例示雙酚A型、溴化雙酚A型、氫化雙酚A型、雙酚F型、雙酚S型、雙酚AF型、聯苯型、萘型、茀型、酚醛清漆型、苯酚酚醛清漆型、鄰甲酚酚醛清漆型、參(羥苯基)甲烷型、四羥苯基乙 烷(tetraphenylol ethane)型等的環氧丙基醚型環氧樹脂。此外，可列舉表氯醇與鄰苯二甲酸衍生物或脂肪酸等羧酸進行縮合所得的環氧丙酯型環氧樹脂，進一步可列舉以各種方法所改質的環氧樹脂，但並不限定於此。特別宜用雙酚型環氧樹脂，其中宜用雙酚A型、雙酚F型的環氧樹脂。
相對於接著劑組成物的總量，含有範圍在1~8質量%的(B)環氧樹脂。若(B)環氧樹脂的含量小於1質量%，接著力會變弱，接續可靠度會降低。反之，若超過8質量%，則不易藉由導電性填充劑的頸縮而形成網絡，而無法得到穩定的導電性、導熱性。(B)環氧樹脂的含量宜為1.4~3.5質量%。
(C)反應性稀釋劑係脂肪族烴鏈中具有2個以上環氧丙基醚官能基且分子量為150~600的化合物。此外，除了環氧丙基醚官能基以外，亦可具有其他聚合性官能基，例如乙烯基、烯丙基等的烯基；丙烯醯基、甲基丙烯醯基等的不飽和基。若分子量小於150，則在進行硬化反應之前，反應性稀釋劑便會揮發而無法得到預定的接著特性；反之，若超過600，反應性稀釋劑的反應性會變慢，而難以得到預期的效果。分子量200~500為更佳。
這種反應性稀釋劑可例舉如：乙二醇二環氧丙基醚、丙二醇二環氧丙基醚、丁二醇二環氧丙基醚、新戊二醇二環氧丙基醚、環己烷二甲醇二環氧丙基醚類的二環氧化物；苯基環氧丙基醚、丁基苯基環氧丙基醚的單環氧化物；三羥甲基丙烷三環氧丙基醚、甘油三環氧丙基醚的三環氧化物等。
其中，從提高本發明之效果的觀點來看，宜為丁二醇二環氧丙基醚、 環己烷二甲醇二環氧丙基醚、丁基苯基環氧丙基醚等為佳。
相對於接著劑組成物的總量，含有範圍在0.2~5質量%的(C)反應性稀釋劑。若(C)反應性稀釋劑的含量小於0.2質量%，樹脂成分會難以分散而變得不均勻，與被接著材料的接合性便會降低。反之，若超過5質量%，硬化後的樹脂會變脆，與被接著材料的接合性降低，且會具有因斷裂等導致導電性降低的疑慮。(C)反應性稀釋劑的含量0.3~1.2質量%為佳。
(D)硬化劑係1分子內具有2個以上酚官能基的化合物、1分子內具有2個以上苯胺官能基的化合物、或該等化合物的混合物。
1分子內具有2個以上酚官能基的化合物可列舉如下列化合物。
式中，R1~R5分別獨立地表示碳數1~5的烷基、烯丙基或氫原子。n表示0以上的整數。
可使用市售品作為這種1分子內具有2個以上酚官能基的化合物，例如，可列舉明和化成股份有限公司製的MEH8000系列(8000H、8005、8010、8015)等。其中，從提高本發明之效果的觀點來看，MEH8000H(上式中，R1~R5為氫或烯丙基，n為0~3的化合物)為佳。
此外，1分子內具有2以上苯胺官能基的硬化劑可列舉如下列 通式(I)、(Ⅱ)或(Ⅲ)所表示之化合物作為較佳例。下列通式(I)、(Ⅱ)或(Ⅲ)所表示之化合物，亦可因應需求組合2種以上。此外，本發明所提及的低級烷基，可列舉碳數1~6之直鏈、分枝或環狀的烷基，碳數1~3之直鏈或分枝的烷基為佳，甲基或乙基為特佳。
特別是下列通式(I)、(Ⅱ)或(Ⅲ)所表示之化合物群之中，式中X為-SO2-的二胺二苯碸及其衍生物，可得到適當的硬化遲延效果，此外，其可促進因導電性填充劑之相互作用所帶來的導電性填充劑之燒結成長及網絡形成，故較宜使用；4,4’-二胺二苯碸及3,3’-二胺二苯碸的效果最強，故最適合使用。此外，在不損及本發明效果下，亦可併用其他習知的硬化劑。
式中，X表示-SO2-、-CH2-或-O-，R1~R4分別獨立地表示氫原子或低級烷基。
式中，X表示-SO2-、-CH2-或-O-，R5~R8分別獨立地表示氫 原子或低級烷基。
式中、X表示-SO2-、-CH2-或-O-，R9~R12分別獨立地表示氫原子或低級烷基。
相對於接著劑組成物的總量，含有範圍在0.2~3質量%的(D)硬化劑。若(D)硬化劑的含量小於0.2質量%，則會有因硬化不充分而耐熱性拙劣的情況。此外，即使在硬化充分的情況下，也會有因為樹脂的硬化速度與導電性填充劑因燒結頸縮而使網絡形成的速度無法適當平衡，而使得導電性或導熱性進而降低的疑慮。反之，若超過3質量%，則由於未反應的硬化劑殘留，而與被接著材料的接合性降低，故不僅電特性降低，也會有因為樹脂的硬化速度與導電性填充劑因燒結頸縮而使網絡形成的速度無法適當平衡，而使得導電性或導熱性進而降低的疑慮。(D)硬化劑的含量0.2~2.5質量%為佳，含量0.3~2質量%為更佳。
本發明中，未表現出與硬化劑之反應性的(E)橡膠系樹脂，其相對於該接著劑組成物的總量，含有範圍在0.2~2質量%為更佳。藉由摻合該(E)橡膠系樹脂，可進一步促進(A)導電性填充劑的頸縮，而能呈現高散熱性。
作為(E)橡膠系樹脂，可舉例如酸改質橡膠。其中，室溫下為液狀的液狀橡膠系樹脂為佳，具有羧基的液狀丙烯腈丁二烯橡膠為更 佳。作為具有羧基的丙烯腈丁二烯橡膠，可列舉下式所表示之化合物。
式中，m表示5~50的整數，a及b分別獨立地表示1以上的整數。a與b的比(a/b)，較佳為95/5~50/50。這種化合物，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(任一皆為宇部興產股份有限公司製)取得。使用CTBN系列為佳。
相對於接著劑組成物的總量，(E)液狀橡膠系樹脂的含量0.2~2質量%為佳，含量0.2~1.5質量%為更佳，0.4~1.1質量%為最佳。
本發明之接著劑組成物，在熱硬化過程中(A)導電性填充劑開始燒結之前，要求其組成物為未硬化或半硬化的狀態。若在熱硬化過程中於(A)導電性填充劑開始燒結之前，接著劑組成物為完全硬化的狀態，則變得無法得到良好的導熱性。
此處，所謂的在熱硬化過程中於(A)導電性填充劑開始燒結之前，係指於使接著劑組成物熱硬化時開始加熱之後，(A)導電性填充劑燒結、平均粒徑增長之前的狀態。此外，接著劑組成物為未硬化的狀態，係指在可溶解該接著劑組成物的溶劑(四氫呋喃)中，實質上完全溶解的狀態。此外，接著劑組成物為半硬化的狀態，係指該接著劑組成物的硬化在中間階段，可說是處於可進行進一步硬化的狀態。半硬化的狀態係一部 分溶解於可溶解接著劑組成物之溶劑(四氫呋喃)中的狀態。
在本發明中，在熱硬化時過程中於(A)導電性填充劑開始燒結之後，該導電性填充劑的平均粒徑成長率到達30%時，接著劑組成物的硬化率特佳為50%以下。若硬化率高於50%，則會有無法得到高導熱性的疑慮。
在本發明中，頸縮係指接著劑組成物的硬化體中的導電性填 充劑彼此之間不單單只有接觸，更有一部分因燒結而處於接續連接的狀態，頸縮率係於200℃下進行1小時的熱處理後，對接著劑組成物之硬化體的垂直剖面進行SEM影像觀察，藉此評估其頸縮之粒子的比例。具體而言，觀察剖面影像大約中心部分30×30μm正方形的影像，並將與各導電性填充劑粒子連接之粒子數(1+連接粒子數)的和除以導電性填充劑粒子數的數值(下式)。例如，觀察影像中具有100個電性填充劑粒子，且與各粒子連接的粒子數共有2個的情況下，與各導電性填充劑粒子連接之粒子的總和為300。此情況下，頸縮率為300%。
[式]頸縮率(%)=100×「1+與各導電性填充劑粒子連接的粒子總和」÷「導電性填充劑粒子數」
本發明中，可藉由使用環氧硬化劑來任意地調節接著劑組成物的硬化率。環氧硬化劑可列舉如：可溶酚醛樹脂型酚醛樹脂(resole phenolic resin)、酚醛清漆型酚醛樹脂(Novolac phenolic resin)、酸酐類、三級胺類、三苯膦類等的硬化觸媒；二氰二醯胺類、聯胺類、芳香族二胺類等的陰離子聚合型硬化劑；有機過氧化物等，但特別宜用可溶酚醛樹脂型酚醛樹脂。可溶酚醛樹脂型酚醛樹脂係由酚類與醛類的反應所產生的樹 脂，其氫氧基具有與環氧基進行反應而使環氧樹脂的分子鏈交聯化而硬化的功能。環氧硬化劑可僅使用一種，亦可併用兩種以上。
可溶酚醛樹脂型酚醛樹脂的摻合量並無限定，因應環氧樹脂的種類或量等而適當決定即可，但使用時相對於本發明之接著劑組成物的總量，一般為0.1~4.0質量%。
本發明之接著劑組成物中亦可摻合硬化促進劑。硬化促進劑可例示如：2-苯基-4,5-二羥甲基咪唑、2-苯基-4-甲基-5-羥甲基咪唑、2-甲基-4-甲基咪唑、1-氰基-2-乙基-4-甲基咪唑等的咪唑類、三級胺類、三苯膦類、尿素系化合物、酚類、醇類、羧酸類等。硬化促進劑可僅使用一種，亦可併用兩種以上。
硬化促進劑的摻合量並無限定，只要適當決定即可，但使用時，相對於本發明之接著劑組成物的總量，一般為0.1~2.0質量%。
本發明之接著劑組成物中亦可摻合溶劑。溶劑可例示如：丁基卡必醇(butyl carbitol)、丁基卡必醇乙酸酯、乙基卡必醇、乙基卡必醇乙酸酯、丁基賽路蘇(butyl cellosolve)、丁基賽路蘇乙酸酯、乙基賽路蘇、乙基賽路蘇乙酸酯、γ-丁內酯、異佛爾酮、環氧丙基苯基醚、三乙二醇二甲醚等的有機溶劑。溶劑可僅使用一種，亦可併用兩種以上。
溶劑的摻合量並無限定，只要適當決定即可，使用時相對於本發明之接著劑組成物的總量，一般為0.1~5.0質量%。
本發明之接著劑組成物中，在不損及本發明之效果的範圍內，亦可適當摻合抗氧化劑、紫外線吸收劑、增黏劑、分散劑、偶合劑、靭性賦予劑、彈性體(elastomer)等作為其他添加劑。
本發明之接著劑組成物係可藉由以任意的順序混合、攪拌上述(A)成分、(B)成分、(C)成分、(D)成分、及因應需求加入之(E)成分與其他成分而得出。分散方法可採用二輥筒、三輥筒、混砂機、輥磨機、球磨機、膠體磨機、噴射磨機、珠磨機、揉合機、均質機、無螺旋槳式混合機等的方式。
此外，本發明之接著劑組成物，在使用(E)成分的情況下，係藉由事先混合(A)成分及(E)成分，之後再混合其他各種成分並進行攪拌，理由雖尚不明確，但藉此可進一步促進(A)導電性填充劑的頸縮，而可得到高導熱性並表現散熱性。
如上述所調製之接著劑組成物中，去除(A)導電性填充劑之情況下的黏度，係藉由旋轉式黏度計進行測定。此外，在本發明中，上述黏度係使用錐板(cone plate)型黏度計作為旋轉式黏度計，於溫度25℃下使用3°×R14錐板，並以特定的轉速(rpm)所測定的值。
此外，如上述所調製之接著劑組成物，去除其中的(A)導電性填充劑的情況下，其由旋轉式黏度計在轉速0.5rpm及5rpm下的測定值所算出TI值(搖變度)係為1~3為佳。藉由具有該TI值，不僅可提高製作漿料(paste)時的作業性，更可發揮以下效果：使電性填充劑與樹脂適當地分散，並促進熱硬化時的導電性填充劑之頸縮化，進而可得到更高導熱性與導電性。此外，在本發明中，上述TI值係由上述旋轉式黏度計的轉速0.5rpm之測定值除以5rpm之測定值所算出的值。
實施例
以下，藉由實施例進一步具體說明本發明，但本發明並不受該等實施例的任何限制。
[實施例1~9、比較例1~3]
A.接著劑組成物的製作
以三個輥筒對表1所記載的各材料進行揉合，以製作表1所示之組成的接著劑組成物(各材料的數值係以相對於接著劑組成物之總質量的質量%來表示)。使用之材料如下所述。此外，揉合的順序是，先進行(A)成分及(E)成分的揉合，接著，混合其他各種成分並揉合使各成分為均勻分散的態樣。於200下加熱1小時後冷卻至室溫，得到接著劑組成物的硬化體。
(A)導電性填充劑
．銀粉[平均粒徑：5.0μm，田中貴金屬工業股份有限公司製]振實密度6.5g/cm3
．銀粉[平均粒徑：1.5μm，田中貴金屬工業股份有限公司製]振實密度4.7g/cm3
．銀粉[平均粒徑：8.0μm，田中貴金屬工業股份有限公司製]振實密度4.2g/cm3
(B)環氧樹脂
．雙酚F型環氧樹脂[EPICRON EXA-830CRP，DIC股份有限公司製，室溫下為液狀]
．苯酚酚醛清漆型環氧樹脂(jER-152，三菱化學股份有限公司製，室溫下為液狀)
．萘型環氧樹脂(DIC股份有限公司製HP4032D，室溫下為液狀)
(C)反應性稀釋劑
．1,4-丁二醇二環氧丙基醚(分子量202.25)
．1,4-環己烷二甲醇二環氧丙基醚(分子量256.34)
(D)硬化劑
．1分子內具有2個以上酚官能基的化合物[明和化成股份有限公司製MEH8000H]
．1分子內具有2個以上苯胺官能基的化合物[東京化成工業股份有限公司製4,4’-二胺二苯碸]
(E)液狀橡膠系樹脂
．具有羧基的丙烯腈丁二烯橡膠[宇部興產股份有限公司製CTBN-1300×13NA]
(硬化促進劑)
．甲苯雙二甲基脲[Carbon Scientific公司製]
．咪唑系硬化促進劑[四國化成工業股份有限公司製2P4MHZ]
(溶劑)
．γ-丁內酯
．N-甲基吡咯啶酮
(其他)
．核殼型粒子[Aica工業股份有限公司製AC-3355]
．矽烷偶合劑(東麗道康寧股份有限公司製Z-6040)
B.接著劑組成物的物性評估
1.黏度
調製將(A)導電性填充劑去除的接著劑組成物，並測定其黏度。黏度係使用錐板型黏度計作為旋轉式黏度計，於溫度25℃下使用3°×R14錐板，以轉速數0.5rpm或5rpm，於溫度25℃下進行測定。結果顯示於表1。
2. TI值
調製將(A)導電性填充劑去除的接著劑組成物，並測定其TI值。TI值係將上述旋轉式黏度計的轉速0.5rpm之測定值除以5rpm之測定值所算出。結果顯示於表1。
3.熱傳導率的測定
為了評估該接著劑組成物的熱傳導特性，測定該接著劑組成物的熱傳導率。熱傳導率λ(W/m．K)，係使用雷射閃光法熱常數測定裝置(TC-7000，ULVAC-RIKO公司製)，根據ASTM-E1461測定熱擴散a，藉由比重計方法算出室溫下的比重d，使用熱示差掃描測定裝置(DSC7020，SEICO電子工業公司製)，根據JIS-K7123測定室溫下的比熱Cp，並以下式算出。結果顯示於表1。
λ=a×d×Cp
4.體積電阻率的測定
為了評估該接著劑組成物的電特性，測定該接著劑組成物的體積電阻率。體積電阻率K(×10-4Ω．cm)係使用直流電壓.發生源監視器(R6243、ADVANTEST公司製)，藉由直流4端子法來測定表觀電阻R，由測定樣本的寬度W、厚度T及長度L，以下式計算得出。結果顯示於表1。
K=L/(R×W×T)
5.頸縮率的測定
以配量器將接著劑組成物塗布於2×2mm正方形的鍍銀之銅製基板上後，以矽製的2×2mm正方形的基板與銅板夾住接著劑組成物的形態進行載置，並於200℃下熱處理1小時後，對接著劑組成物之硬化體的垂直剖面進行SEM影像觀察，藉此評估頸縮率。具體而言，係對接著劑組成物之硬化體的剖面影像大約中心部位的任意5處，分別觀察30×30μm正方形的影像，並將與各導電性填充劑粒子連接之粒子數(1+連接粒子數)的和除以導電性填充劑粒子數的數值(下式)的平均值所算出。算出結果顯示於表1。
[式]頸縮率(%)=100×「1+與各導電性填充劑粒子連接的粒子總和」÷「導電性填充劑粒子數」
由上述結果可確認，本發明之接著劑組成物具有高熱傳導率與穩定的導電性。
雖參照特定的態樣詳細說明本發明，但只要不脫離本發明之宗旨與範圍，可進行各種變更及修正，此為本領域具有通常知識者明確可知。
此外，本申請案係根據2014年5月29日提出申請之日本專利申請(特願2014-111769)，將其所有內容引用至本文。

Claims (3)

  1. 一種導熱性導電性接著劑組成物，其係包含(A)導電性填充劑、(B)環氧樹脂、(C)反應性稀釋劑及(D)硬化劑，其中：該(A)導電性填充劑係具有平均粒徑1~10μm的銀粉，且相對於該導熱性導電性接著劑組成物的總量，該(A)導電性填充劑的含量為85~94質量%的範圍；該(B)環氧樹脂係1分子內具有2個以上環氧官能基及芳香環，且相對於該導熱性導電性接著劑組成物的總量，該(B)環氧樹脂的含量為1~8質量%的範圍；該(C)反應性稀釋劑係於脂肪族烴鏈中具有2個以上環氧丙基醚官能基且分子量為150~600的化合物，且相對於該導熱性導電性接著劑組成物的總量，該(C)反應性稀釋劑的含量為0.2~5質量%的範圍；且該(D)硬化劑係1分子內具有2以上之酚官能基的化合物、1分子內具有2以上之苯胺官能基的化合物、或該等化合物的混合物，且相對於該導熱性導電性接著劑組成物的總量，該(D)硬化劑的含量為0.2~3質量%的範圍。
  2. 如申請專利範圍第1項之導熱性導電性接著劑組成物，其中進一步包含未表現出與該(D)硬化劑之反應性的(E)橡膠系樹脂，且相對於該導熱性導電性接著劑組成物的總量，該(E)橡膠系樹脂的含量為0.2~2質量%的範圍。
  3. 如申請專利範圍第1項之導熱性導電性接著劑組成物，其中將該導熱 性導電性接著劑組成物中的該(A)導電性填充劑去除的組成物，其由旋轉式黏度計在旋轉數0.5rpm及5rpm下的測定值所算出的TI值(搖變度)為1~3。
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