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TW201542758A - 導電性組合物及導電性成形體 - Google Patents

導電性組合物及導電性成形體 Download PDF

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Publication number
TW201542758A
TW201542758A TW104105899A TW104105899A TW201542758A TW 201542758 A TW201542758 A TW 201542758A TW 104105899 A TW104105899 A TW 104105899A TW 104105899 A TW104105899 A TW 104105899A TW 201542758 A TW201542758 A TW 201542758A
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Taiwan
Prior art keywords
conductive
resin
group
metal
composition
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Application number
TW104105899A
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English (en)
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TWI613272B (zh
Inventor
Taisuke Iseda
Masahiro Iwamoto
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Mitsuboshi Belting Ltd
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Publication of TW201542758A publication Critical patent/TW201542758A/zh
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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
    • C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
    • C09J9/02—Electrically-conducting adhesives
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • 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
    • C08G59/20—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 epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
    • C08G59/245—Di-epoxy compounds carbocyclic aromatic
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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
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    • C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/08—Materials not undergoing a change of physical state when used
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    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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Abstract

本發明係關於一種導電性組合物，其係包含導電性金屬粉及樹脂成分之組合物，且導電性金屬粉至少包含具有金屬結晶成長為薄片狀之晶體結構之金屬薄片，上述樹脂成分包含芳香族胺骨架。

Description

導電性組合物及導電性成形體
本發明係關於一種對於形成導電性接著劑、電極等有用之導電性組合物、及包含由該導電性組合物所形成之導電性部位(導電性接著層、電極、配線等)之成形體(導電性成形體)。
包含銀膏等導電性金屬粉(導電性填料)之導電性組合物(導電膏)一直被用於形成電子零件等之電極或電路。其中包含熱塑性或熱硬化性樹脂之導電膏通常藉由使用之樹脂之收縮而使導電性填料彼此接觸而表現導電性，又，藉由存在樹脂(黏合劑)而保證對基材之密接性或接著性。因此，於包含此種黏合劑之導電膏中，為了獲得充分之導電性，增大導電性金屬粉間之接觸面積變得重要。就此種觀點而言，作為導電性金屬粉，正嘗試使用金屬薄片(薄片狀金屬粉)。
例如，於日本專利特開2008-171828號公報(專利文獻1)中揭示有包含薄片狀之銀粉及有機樹脂之導電膏。該文獻中，作為有機樹脂，廣泛例示有聚酯樹脂、改性聚酯樹脂(胺基甲酸酯改性聚酯樹脂等)、聚醚胺基甲酸酯樹脂、聚碳酸酯胺基甲酸酯樹脂、氯乙烯-乙酸乙烯酯共聚物、環氧樹脂、酚樹脂、丙烯酸系樹脂、聚醯胺醯亞胺、硝化纖維素、纖維素-乙酸酯-丁酸酯、纖維素-乙酸酯-丙酸酯等有機樹脂，特別是於實施例中，根據耐撓曲性等觀點使用聚酯樹脂及胺基甲酸酯改性聚酯樹脂。
又，於日本專利特開2012-92442號公報(專利文獻2)中揭示有平 均粒徑與BET(Brunauer-Emmett-Teller，布厄特)比表面積有特定關係之薄片狀銀粉。而且，於該文獻中，作為用於導電膏之樹脂，例示有環氧樹脂、丙烯酸系樹脂、聚酯樹脂、聚醯亞胺樹脂、聚胺基甲酸酯樹脂、苯氧基樹脂、聚矽氧樹脂等，於實施例中使用聚酯樹脂。
此種導電膏雖顯示出一定程度之導電性，但期待進一步之導電性或接著性之改善。
[先前技術文獻] [專利文獻]
[專利文獻1]日本專利特開2008-171828號公報(申請專利範圍，段落[0014]~[0022]，實施例)
[專利文獻2]日本專利特開2012-92442號公報(申請專利範圍，段落[0026]，實施例)
因此，本發明之目的在於提供一種即便包含樹脂成分亦可實現優異之導電性之導電性組合物、及具有由該導電性組合物所形成之導電性部位之成形體。
本發明之另一目的在於提供一種可於無損對基材之密接性或接著性之情況下改善或提昇導電性之導電性組合物、及具有由該導電性組合物所形成之導電性部位之成形體。
本發明之進而另一目的在於提供一種導電性及放熱性優異之導電性接著劑、及具備藉由該導電性接著劑直接接著之接合基材之成形體。
本發明者等人為了解決上述課題進行了銳意研究，結果發現：藉由於導電性組合物中將金屬薄片(薄片狀金屬粉)及特定之樹脂成分 加以組合，可獲得較高之導電性，可同時實現較高之導電性、及對基材之優異之密接性或接著性，進而即便於要求較高之放熱性之導電性接著劑用途等中，亦可保證充分之導電性及放熱性(進而密接性)，從而完成本發明。
即，本發明之導電性組合物係包含導電性金屬粉及樹脂成分之組合物，且導電性金屬粉包含金屬薄片，樹脂成分包含芳香族胺骨架(或芳香族胺或源自芳香族胺之骨架)。再者，所謂「具有芳香族胺骨架之樹脂成分」，意指於經硬化或固化之狀態下具有芳香族胺骨架或殘基(特別是芳香族聚胺骨架或殘基)之樹脂成分，不僅包含使用芳香族胺(特別是芳香族聚胺)作為反應成分之樹脂，亦包含包含樹脂及芳香族胺(特別是芳香族聚胺)之樹脂組合物。
於此種組合物中，金屬薄片至少包含具有金屬(或金屬結晶)薄片狀地(或二維地)成長(或晶體成長)之晶體結構之金屬薄片。例如，於將X射線繞射之(111)面、(200)面之繞射積分強度分別設為I111、I200時，上述金屬薄片可為下述式所表示之值X為30%以下(例如20%以下)之金屬薄片。
X=[I200/(I111+I200)]×100(%)
上述樹脂成分可為熱硬化性樹脂成分。於代表性態樣中，樹脂成分為包含熱硬化性樹脂(或熱硬化性樹脂前驅物)及硬化劑(或交聯劑)之熱硬化性樹脂組合物，熱硬化性樹脂及/或硬化劑可包含芳香族胺骨架。於此種熱硬化性樹脂組合物中，硬化劑可包含芳香族胺系硬化劑。更具體而言，樹脂成分可為包含作為熱硬化性樹脂之環氧樹脂(例如環氧當量為600g/eq以下之環氧樹脂)、及硬化劑(包含芳香族胺系硬化劑)之環氧樹脂組合物。芳香族胺系硬化劑例如可為具有芳香環上直接取代有胺基之結構之芳香族胺系硬化劑。
硬化劑亦可包含下述式(1)所表示之芳香族聚胺。
(式中，環Z分別獨立，表示芳烴環，A表示伸烷基或亞烷基、伸環烷基或亞環烷基、伸芳基、氧原子、硫原子、亞磺醯基、或磺醯基，R表示烷基、環烷基、芳基、芳烷基、烷氧基、或鹵素原子，m表示0或1，n分別獨立，表示0~4之整數)
關於樹脂成分之比率，相對於金屬薄片100重量份，例如可為1~50重量份左右。
本發明之導電性組合物可為導電性接著劑(例如黏晶膏)，例如用以使金屬基材與半導體基材接著之導電性接著劑。
於本發明中，亦包含至少具有由上述導電性組合物所形成之導電性部位(或導電膜)之成形體(導電性成形體、導電性構件)。此種成形體(電氣、電子零件等)係具備由2片基材、及介存於該基材間且使2片基材接著之導電性接著劑所構成之接合基材的成形體(或接合構件)，可為導電性接著劑為由上述導電性組合物所形成之導電性部位之成形體(或接合構件)。此種成形體例如可由金屬基材(引線框架等)、半導體基材(搭載有半導體晶片等電子零件之基材等)、及介存於該等基材間且使兩者接著之上述導電性組合物(或接著層)而形成。
進而，本發明亦包含藉由上述X射線繞射而得之導電性部位之上述值X為30%以下(例如20%以下)之導電性成形體。
本發明之導電性組合物不論是否包含作為黏合劑之樹脂成分均 可實現優異之導電性。而且，可於無損對基材之密接性或接著性之情況下實現較高之導電性。又，本發明之導電性組合物由於導電性及放熱性(熱傳導性)亦優異，故而作為導電性接著劑有用。
<導電性組合物>
本發明之導電性組合物以特定之導電性金屬粉及特定之樹脂成分而構成。
[導電性金屬粉]
導電性金屬粉至少包含金屬薄片(薄片狀金屬粉、板狀金屬粉、鱗片狀金屬粉)。
(金屬薄片)
作為構成金屬薄片之金屬(金屬原子)，例如可列舉：過渡金屬(例如：鈦、鋯等週期表第4族金屬；釩、鈮等週期表第5族金屬；鉬、鎢等週期表第6族金屬；錳、錸等週期表第7族金屬；鐵、鎳、鈷、釕、銠、鈀、銥、鉑等週期表第8~10族金屬；銅、銀、金等週期表第11族金屬等)、週期表第12族金屬(例如：鋅、鎘等)、週期表第13族金屬(例如：鋁、鎵、銦等)、週期表第14族金屬(例如：鍺、錫、鉛等)、週期表第15族金屬(例如：銻、鉍等)等。金屬可單獨使用或將2種以上組合。
金屬除可為金屬單質外，亦可為金屬之合金或金屬與非金屬之化合物(例如：金屬氧化物、金屬氫氧化物、金屬硫化物、金屬碳化物、金屬氮化物、金屬硼化物等)之形態。通常，金屬為金屬單質或金屬合金之情況較多。代表性金屬包含週期表第8~10族金屬(鐵、鎳、銠、鈀、鉑等)、週期表第11族金屬(銅、銀、金等)、週期表第13 族金屬(鋁、銦等)、週期表第14族金屬(錫等)、及該等之合金等。金屬尤佳為至少包含銀等貴金屬(特別是週期表第11族金屬)之金屬(例如：金屬單質、金屬合金)，特別是貴金屬單質(例如：銀單質等)。由該等金屬所形成之薄片可單獨使用或將兩種以上組合使用。
金屬薄片為(i)具有金屬(或金屬結晶)薄片狀地(或二維地)成長(或晶體成長)之晶體結構(晶體結構1)之金屬薄片、(ii)具有集成有大量微晶之晶體結構(晶體結構2)之金屬微粒子(或球狀微粒子)之薄片化(或扁平化)物等之任一者均可。金屬薄片至少包含上述金屬薄片(i)。
再者，金屬薄片(i)主要具有使結晶單質成長而成長為薄片狀之金屬之晶體結構，相對於此，金屬薄片(ii)通常係將具有集成有大量微晶之晶體結構之金屬微粒子(或其凝聚物)進行薄片化(或扁平化)，故而薄片化物亦又成為主要具有集成有大量微晶之晶體結構。又，金屬薄片(ii)由於係物理地進行薄片化，故而於金屬表面容易生成微細之凹凸。
主要具有晶體結構1之金屬薄片(i)存在如下情況：雖然與晶體結構2相比因晶界之電阻較小而較佳，但於結晶面之中占薄片之大部分面積之板面[例如，於為如銀薄片之面心立方晶格之情形時主要為(111)面]之表面能較低，界面之金屬鍵亦不易產生，故而變得無法保證充分之導電性。另一方面，金屬薄片(ii)雖然因晶體結構2而與晶體結構1相比晶界之電阻變大，但或許因表面之微細之凹凸，與晶體結構1相比，金屬薄片界面之燒結性變大，亦可期待藉由金屬鍵之低電阻化。
就此種觀點而言，金屬薄片根據所需用途或導電性等適當選擇即可，本發明中尤其可較佳地使用金屬薄片(i)。即便為此種金屬薄片(i)，或許由於藉由與樹脂成分組合可確保金屬薄片彼此之充分之接觸，亦可保證較高之導電性，進而，該等成分進行協同作用，與使用 金屬薄片(ii)之情形相比，可實現更高之導電性。
再者，金屬薄片之結晶性之程度可將X射線繞射之繞射強度作為指標進行估計。若利用粉末X射線繞射法，於具有藉由晶體成長而賦予有各向異性(配向性)之晶體結構1之金屬薄片中，對平面或板面之繞射主要對應於(111)面，並以較大之強度而表現，對形成厚度之面之繞射主要對應於(200)面，其強度表現極小。另一方面，於集成有大量微晶之金屬薄片(ii)中，各向異性(配向性)較小，自(111)面、(200)面之繞射強度之差異變小。因此，變為(111)面之強度越大，且(200)面之強度越小，晶體結構1之比率越大。具體而言，於將X射線繞射(2θ/θ掃描法)之(111)面及(200)面之繞射積分強度分別設為I111及I200時，可將下述式所表示之值X成為30%以下(例如0~25%)、較佳為20%以下(例如0~18%)、進而較佳為15%以下(例如0~12%)、特別是10%以下(例如0~9%)之金屬薄片設為主要具有晶體結構1之金屬薄片(即金屬薄片(i))。值X例如可為1~10%，較佳為2~7.5%左右。再者，有時將藉由上述X射線繞射而獲得之值X僅稱為「值X」。
X=[I200/(I111+I200)]×100(%)
若使用此種金屬薄片，則即便於成形後(例如將導電性組合物進行硬化處理之後)，亦可形成維持上述X之值之(或保持金屬薄片之結晶狀態之)導電性部位或導電性接著劑，且可形成較高之導電性之導電性成形體。
再者，於金屬薄片(ii)中，上述值X可為超過25%(例如27~40%)，較佳為30%以上(例如32~40%)左右，通常可為27~35%左右。
金屬薄片可使用市售品，亦可藉由慣用之方法進行製備。例如，金屬薄片(i)可使用日本專利第3429985號公報、日本專利第4144856號公報、日本專利第4399799號公報、日本專利特開2009- 144188號公報等記載之製造方法進行合成，且可使用該等文獻記載之金屬薄片。又，金屬薄片(ii)可使用上述專利文獻1或2記載之方法進行合成。
金屬薄片之平均粒徑例如可為0.1~20μm，較佳為0.3~15μm(例如0.5~12μm)，進而較佳為0.7~10μm(例如0.8~7μm)左右，通常可為1~10μm左右。再者，金屬薄片之平均粒徑例如可利用雷射繞射散射式粒度分佈測定法等進行測定。若利用此種測定法，平均粒徑(中心粒徑)可作為體積基準之值而測定。
金屬薄片之平均厚度例如可為5~1000nm，較佳為20~500nm，進而較佳為50~300nm，通常可為10~300nm左右。
又，金屬薄片之縱橫比(平均粒徑/平均厚度)例如可為5~100，較佳為7~50，進而較佳為10~30左右。
金屬薄片之BET比表面積可自0.3~7m2/g左右之範圍進行選擇，例如可為0.5~6m2/g，較佳為1~5m2/g，進而較佳為1.2~4m2/g左右，通常可為1~5m2/g左右。
金屬薄片之搖實密度可自0.1~7g/cm3(例如0.2~6g/cm3)左右之範圍進行選擇，例如可為0.3~5g/cm3，較佳為0.5~4.5g/cm3，進而較佳為1~4g/cm3左右，通常可為1.2~4g/cm3(例如1.5~3.5g/cm3)左右。
(金屬粒子)
於本發明之組合物中，為了對導電性、流動性進行調整，金屬薄片可與上述X值大於20%之金屬粒子組合使用。藉由與金屬粒子組合，可對導電性、膏之流動性進行調整。金屬粒子之形態可為X值大於20%之粒子，亦可為球狀、纖維狀等。再者，形成金屬粒子之金屬與上述相同，可與金屬薄片同種或異種。金屬粒子可單獨使用或將2種以上組合。再者，金屬粒子可使用市售品，亦可藉由慣用之方法進 行製備。
再者，金屬薄片之平均粒徑與金屬粒子之平均粒徑之比率(比)例如可為前者/後者=2/1~1000/1(例如3/1~500/1)，較佳為4/1~300/1(例如5/1~200/1)，進而較佳為10/1~100/1左右。金屬粒子之平均粒徑亦可例如利用雷射繞射散射式粒度分佈測定法等進行測定。
金屬薄片與金屬粒子(球狀金屬粒子等)之比率可自前者/後者(重量比)=100/0~5/95(例如99/1~10/90)左右之範圍進行選擇，例如可為95/5~25/75(例如90/10~30/70)，較佳為85/15~40/60(例如80/20~45/55)左右，亦可為99/1~30/70左右。
[樹脂成分]
於本發明中，構成導電性組合物之樹脂成分具有芳香族胺骨架(或源自芳香族胺之骨架)。藉由將金屬薄片與具有芳香族胺骨架之樹脂成分加以組合，可實現較高之導電性，且可保證對基板之充分之密接性。此種原因雖不確定，但除存在具有芳香族胺骨架之樹脂成分會促進金屬薄片彼此之接觸或燒結(金屬鍵之形成)之情況以外，亦可推斷為硬化或固化後所形成之剛性之具有芳香族胺骨架之樹脂結構、與由金屬薄片所形成之剛性之金屬網狀結構之配合性良好。
具有芳香族胺骨架之樹脂成分只要為硬化或固化之狀態且具有芳香族胺骨架或殘基(特別是包含芳香族二胺之芳香族聚胺骨架或殘基)之樹脂成分即可，亦包含(a)使用芳香族胺(特別是包含芳香族二胺之芳香族聚胺)作為反應成分(聚合成分、或改質(或改性)成分)之樹脂，(b)包含樹脂、及與該樹脂進行反應之成分[例如與熱硬化性樹脂進行反應之硬化劑(例如包含芳香族胺(特別是包含芳香族二胺之芳香族聚胺)系硬化劑之硬化劑)]之樹脂組合物。
上述樹脂(a)根據樹脂之態樣而包含芳香族胺骨架或殘基，芳香族胺之胺基可形成游離之胺基(或亞胺基)。
上述樹脂(a)為熱塑性樹脂、熱硬化性樹脂之任一者均可。作為熱塑性樹脂，可列舉：以芳香族胺作為聚合成分(或單體)之樹脂[例如：使用有包含芳香族二胺(後述芳香族胺系硬化劑等)之二胺成分之聚醯胺樹脂；以具有芳香族胺骨架之自由基聚合性單體(例如：(甲基)丙烯酸2-乙基胺基苯酯、(甲基)丙烯酸4-(苯甲醯基胺基)苯酯等)作為聚合成分之加成聚合系樹脂((甲基)丙烯酸系樹脂等)等]等。又，熱塑性樹脂亦可為將對胺基具有反應性之熱塑性樹脂利用芳香族胺(特別是芳香族聚胺)進行改質或改性而成之樹脂。作為上述對胺基具有反應性之熱塑性樹脂，可例示：具有羧基之樹脂(以(甲基)丙烯酸等含羧基聚合性單體作為聚合成分之(甲基)丙烯酸系均聚或共聚物、具有羧基或酸酐基之聚酯樹脂等)、具有環氧基之樹脂(以(甲基)丙烯酸縮水甘油酯作為聚合成分之(甲基)丙烯酸系均聚或共聚物等)、具有異氰酸酯基之樹脂(胺基甲酸酯系樹脂等)等。該等熱塑性樹脂可單獨使用或將兩種以上組合使用。
較佳之樹脂(a)為熱硬化性樹脂，作為熱硬化性樹脂，可例示以芳香族胺(二胺等芳香族聚胺)作為聚合成分(或單體)之樹脂，例如縮水甘油胺型芳香族環氧樹脂、苯胺樹脂、酚樹脂(共縮合有苯胺等芳香族胺之酚樹脂等)、胺基樹脂(共縮合有苯胺等芳香族胺之胺基樹脂等)等。
進而，具有芳香族胺骨架之樹脂成分較佳為上述樹脂組合物(b)，該樹脂組合物(b)之樹脂較佳為熱硬化性樹脂。即，上述樹脂組合物(b)包含熱硬化性樹脂(或熱硬化性樹脂前驅物)及硬化劑(或交聯劑)，且熱硬化性樹脂及/或硬化劑包含芳香族胺骨架。尤佳為由熱硬化性樹脂、及包含芳香族胺系硬化劑之硬化劑構成熱硬化性樹脂組合物。若使用芳香族胺系硬化劑，則可更高效地實現較高之導電性。其原因雖不明確，但認為係因金屬薄片與芳香族胺骨架之相互作用而使 導電性提昇。
於使用上述樹脂(a)所例示之樹脂作為樹脂組合物(b)之熱硬化性樹脂之情形時，作為硬化劑，可例示對胺基具有反應性之慣用之硬化劑，例如酸酐系硬化劑、異氰酸酯系硬化劑等。作為樹脂組合物(b)之熱硬化性樹脂，除上述樹脂(a)所例示之樹脂以外，例如還可例示：環氧樹脂、酚樹脂、聚胺基甲酸酯樹脂(具有異氰酸酯基之聚異氰酸酯樹脂)、(甲基)丙烯酸系樹脂或苯乙烯系樹脂(具有羧基或酸酐基、縮水甘油基、異氰酸酯基之(甲基)丙烯酸系樹脂或苯乙烯系樹脂等)、聚醯亞胺樹脂(具有酸酐基之聚醯胺酸等)等。該等熱硬化性樹脂可單獨使用或將2種以上組合。於此情形時，作為硬化劑，可使用後述包含芳香族胺系硬化劑之硬化劑。例如，樹脂組合物(b)可為包含聚異氰酸酯化合物(或具有異氰酸酯基之聚異氰酸酯樹脂)、及硬化劑(包含芳香族胺系硬化劑)之聚異氰酸酯樹脂組合物，亦可為包含環氧樹脂、及硬化劑(包含芳香族胺系硬化劑)之環氧樹脂組合物。
再者，於具有芳香族胺骨架之樹脂成分為上述樹脂(a)時，芳香族胺骨架(源自芳香族胺之骨架)之比率例如可為樹脂成分整體之1重量%以上(例如2~100重量%)，較佳為3重量%以上(例如5~90重量%)，進而較佳為5重量%以上(例如10~80重量%)左右。
於具有芳香族胺骨架之樹脂成分為樹脂組合物(b)時，芳香族胺骨架相對於樹脂成分整體之比率(例如芳香族胺系硬化劑之比率)可為樹脂成分整體之1重量%以上(例如2~80重量%)，較佳為5~50重量%，進而較佳為10~30重量%左右。再者，芳香族胺系硬化劑之比率例如相對於熱硬化性樹脂100重量份可為0.1~500重量份，較佳為1~300重量份，進而較佳為3~150重量份，特別是5~100重量份左右。
以下，作為較佳之熱硬化性樹脂組合物，針對包含環氧樹脂作為主劑、包含芳香族胺系硬化劑作為硬化劑之樹脂組合物進行說明。
(環氧樹脂)
環氧樹脂通常至少包含多官能環氧樹脂，多官能環氧樹脂例如為縮水甘油醚型、縮水甘油胺型、縮水甘油酯型、脂環式型等任一者均可。多官能環氧樹脂亦可為脂肪族環氧樹脂、脂環族環氧樹脂、芳香族環氧樹脂、含氮型環氧樹脂(含氮型多官能環氧樹脂，例如三縮水甘油基異氰尿酸酯等)等。於多官能環氧樹脂中，分子中之環氧基之數量根據環氧樹脂之種類可為2以上，例如2~150(例如2~100)，較佳為2~80(例如2~50)，進而較佳為2~30左右。環氧樹脂可單獨使用或將2種以上組合。
作為脂肪族環氧樹脂中之二縮水甘油醚型環氧樹脂，例如可例示：烷烴多元醇聚縮水甘油醚(丁二醇、新戊二醇等烷烴二醇；聚乙二醇、聚丙二醇等聚C2-4烷烴二醇；選自三羥甲基丙烷、甘油、季戊四醇等烷烴三至六醇中之烷烴多元醇之二至六縮水甘油醚等)、環己烷二甲醇二縮水甘油醚等。作為縮水甘油酯型環氧樹脂，可例示環烷烴二羧酸(1,2-環己烷二羧酸、1,3-環己烷二羧酸、1,4-環己烷二羧酸等)、二聚酸縮水甘油酯等。
作為脂環族環氧樹脂，例如可例示烷烴多元醇與環氧環烷烴羧酸之酯(例如：3,4-環氧環己基甲基-3,4-環氧環己烷羧酸酯；2,2-雙(羥甲基)-1-丁醇與3,4-環氧環己烷羧酸之三酯等)等。
芳香族環氧樹脂包含縮水甘油醚型芳香族環氧樹脂、縮水甘油酯型芳香族環氧樹脂、縮水甘油胺型芳香族環氧樹脂。
作為縮水甘油醚型芳香族環氧樹脂，例如可例示：芳烴縮水甘油醚類[例如：二縮水甘油氧基苯類、二縮水甘油氧基萘(例如：2,6-二(縮水甘油氧基)萘、2,7-二(縮水甘油氧基)萘等聚縮水甘油氧基萘類)、4,4'-二縮水甘油氧基聯苯、2,2'-二縮水甘油氧基聯萘等]；雙酚型環氧樹脂；酚醛清漆型環氧樹脂等。
作為雙酚型環氧樹脂，可列舉雙酚類或其環氧烷(例如：環氧乙烷、環氧丙烷等C2-4環氧烷)加成體之二縮水甘油醚。作為雙酚類，例如可列舉：聯苯酚、聯萘酚等聯(羥基芳烴)類；雙酚A、雙酚B、雙酚E、雙酚F等雙(羥基苯基)C1-10烷烴；2,2-雙(3-甲基-4-羥基苯基)丙烷、雙酚G等雙(C1-10烷基-羥基苯基)C1-10烷烴；雙酚PH等雙(羥基C6-10芳基苯基)C1-10烷烴；雙酚Z、雙酚TMC等雙(羥基苯基)C5-10環烷烴；雙酚AP、雙酚BP；雙酚AF；雙酚S；雙酚M；雙酚P；雙萘酚類(例如：1,1'-亞甲基雙(羥基萘)等雙(羥萘基)C1-10烷烴)等。再者，於雙酚類之環氧烷加成體中，環氧烷相對於雙酚類之羥基1莫耳之加成莫耳數例如可為1莫耳以上(例如1~20莫耳)，較佳為1~15莫耳，進而較佳為1~10莫耳左右。
作為酚醛清漆型環氧樹脂，可列舉以酚類作為聚合成分之酚醛清漆樹脂之縮水甘油醚。作為酚類，例如可列舉：苯酚；烷酚(例如：甲酚、乙基苯酚、第二丁基苯酚、第三丁基苯酚、癸基苯酚、十二烷基苯酚等C1-12烷酚，較佳為C1-4烷酚)、芳烷基苯酚(例如1,1-二甲基-1-苯基甲基苯酚等C6-10芳基C1-10烷酚)等取代苯酚；萘酚類(例如萘酚等)、雙酚類(上述例示之雙酚類)等。該等酚類可單獨或將2種以上組合而構成酚醛清漆樹脂。
作為代表性之酚醛清漆型環氧樹脂，例如可列舉：苯酚酚醛清漆型環氧樹脂、烷酚酚醛清漆型環氧樹脂(例如甲酚酚醛清漆型環氧樹脂等)、萘酚酚醛清漆型環氧樹脂、雙酚酚醛清漆型環氧樹脂(例如：雙酚A酚醛清漆型環氧樹脂、雙酚F酚醛清漆型環氧樹脂等)、改性酚醛清漆型環氧樹脂[例如：芳烷基酚醛清漆型環氧樹脂(例如含有苯二甲基骨架之苯酚酚醛清漆型樹脂等)、含有二環戊二烯骨架之酚醛清漆型環氧樹脂(例如含有二環戊二烯骨架之苯酚酚醛清漆型環氧樹脂)、含有聯苯骨架之酚醛清漆型環氧樹脂(例如含有聯苯骨架之苯 酚酚醛清漆型環氧樹脂)、溴化酚醛清漆型環氧樹脂(例如溴化苯酚酚醛清漆型環氧樹脂)等]等。
再者，酚醛清漆型環氧樹脂之數量平均分子量例如可為1000~1000000，較佳為2000~100000，進而較佳為3000~25000左右。
作為縮水甘油酯型芳香族環氧樹脂，例如可例示：芳香族二羧酸(鄰苯二甲酸、間苯二甲酸、對苯二甲酸、萘二甲酸等)之二縮水甘油酯等。
作為縮水甘油胺型芳香族環氧樹脂，例如可列舉：N,N-二縮水甘油基苯胺；四縮水甘油基二胺基二苯甲烷、四縮水甘油基間苯二甲胺等四至八縮水甘油基聚胺；三縮水甘油基對胺基苯酚；N,N-二縮水甘油基-4-縮水甘油氧基苯胺(或N,N-雙(2,3-環氧丙基)-4-(2,3-環氧丙氧基)苯胺)等。
環氧樹脂之環氧當量並無特別限定，可自800g/eq以下(例如50~750g/eq)左右之範圍進行選擇，例如可為700g/eq以下(例如70~650g/eq)，較佳為600g/eq以下(例如80~550g/eq)，特別是500g/eq以下(例如100~450g/eq)左右。
環氧樹脂可為單官能環氧樹脂。單官能環氧樹脂用作反應性稀釋劑之情況較多。作為單官能環氧樹脂，例如可例示：縮水甘油醚類(例如：苯基縮水甘油醚、鄰苯基苯基縮水甘油醚等芳香族單縮水甘油醚)、環烯烴氧化物類(例如4-乙烯基環氧環己烷、環氧六氫苯二甲酸二烷基酯等)等。
再者，多官能環氧樹脂與單官能環氧樹脂之比率可自前者/後者(重量比)=100/0~30/70左右之範圍進行選擇，例如可為99/1~40/60(例如97/3~50/50)，較佳為95/5~60/40(例如95/5~70/30)左右。
(芳香族胺系硬化劑)
作為芳香族胺系硬化劑，可例示二胺等芳香族聚胺，例如：對 苯二胺、間苯二胺等二胺基C6-10芳烴；甲苯二胺等二胺基-單至三C1-4烷基C6-10芳烴；苯二甲胺等二(胺基C1-4烷基)C6-10芳烴等，此外下述式(1)所表示之芳香族聚胺(雙芳基聚胺)等。
(式中，環Z分別獨立，表示芳烴環，A表示伸烷基或亞烷基、伸環烷基或亞環烷基、伸芳基、氧原子、硫原子、亞磺醯基、或磺醯基，R表示烷基、環烷基、芳基、芳烷基、烷氧基、或鹵素原子，m表示0或1，n分別獨立，表示0~4之整數)
作為環Z所表示之芳烴環，可例示苯環、萘環等C6-10芳烴環。環Z為苯環之情況較多。作為A所表示之伸烷基或亞烷基，可例示：亞甲基、伸乙基、亞乙基、伸丙基、2-亞丙基、2-亞丁基等直鏈狀或支鏈狀C1-6伸烷基或亞烷基。該等伸烷基或亞烷基可被芳基(苯基等之C6-10芳基)、鹵素原子等取代。作為伸環烷基或亞環烷基，可例示1,4-伸環己基、亞環己基等C4-10伸環烷基或亞環烷基等，作為伸芳基，可例示伸苯基等C6-10伸芳基、4,4'-聯伸苯基、茀-9,9-二基等。A可為氧原子或醚基(-O-)、硫原子或硫基(-S-)、亞磺醯基(-SO-)、磺醯基(-SO2-)。
係數m為0或1，m=0之化合物形成聯芳基化合物。
作為R所表示之烷基，可例示甲基、乙基等C1-6烷基。作為環烷基，可例示環己基等C5-8環烷基，作為芳基，可例示苯基等C6-10芳基，作為芳烷基，可例示苄基等C6-8芳基-C1-2烷基等。作為烷氧基， 可例示甲氧基、乙氧基、丁氧基等C1-6烷氧基等。鹵素原子包含氟、氯、溴原子等。較佳之R為烷基(甲基等C1-4烷基)。再者，於存在複數個取代基R之情形時，取代基R之種類可相同或不同。
係數n可自0~4之整數進行選擇，通常可為0~2(例如1或2)。
再者，於環Z為苯環時，胺基鍵結於3-位或4-位(特別是4-位)之情況較多，取代基R鍵結於3-位、4-位及/或5-位(特別是3-位及/或5-位)之情況較多。
作為上述式(1)所表示之雙芳基聚胺，例如可例示：二胺基聯芳烴(4,4'-二胺基聯苯等)；雙(胺基芳基)烷烴(例如二(4-胺基苯基)甲烷等二(胺基C6-10芳基)C1-6烷烴)；雙(胺基-烷基芳基)烷烴(例如雙(3-乙基-4-胺基苯基)甲烷、雙(3-乙基-5-甲基-4-胺基苯基)甲烷等二(胺基-C1-4烷基C6-10芳基)C1-6烷烴)；雙(胺基芳基)醚(例如二胺基二苯基醚等二(胺基C6-12芳基)醚，較佳為二(胺基C6-10芳基)醚等)；雙(胺基芳基)硫醚(例如二胺基二苯基硫醚等二(胺基C6-12芳基)硫醚，較佳為二(胺基C6-10芳基)硫醚等)；雙(胺基芳基)碸(例如二胺基二苯基碸等二(胺基C6-12芳基)碸，較佳為二(胺基C6-10芳基)碸等)；雙(胺基芳基烷基)芳烴(例如：1,3-雙[2-(4-胺基苯基)-2-丙基]苯、1,4-雙[2-(4-胺基苯基)-2-丙基]苯等雙(胺基C6-10芳基C1-10烷基)C6-10芳烴等)；二(胺基芳氧基)芳烴(例如1,3-雙(3-胺基苯氧基)苯等二(胺基C6-12芳氧基)C6-12芳烴，較佳為二(胺基C6-10芳氧基)C6-10芳烴)等。
該等芳香族胺系硬化劑可單獨使用或將2種以上組合。作為較佳之硬化劑，可例示雙酚系聚胺，特別是式(1)所表示之化合物，例如芳香環上直接取代胺基之芳香族胺[例如：聚(胺基芳基)烷烴、二(胺基芳基)醚、二(胺基芳基)碸等]等。
再者，芳香族胺系硬化劑若有必要則可與其他硬化劑組合。作為其他硬化劑，例如可列舉：脂肪族胺系硬化劑(例如：乙二胺、六 亞甲基二胺、二伸乙基三胺、三伸乙基四胺、四伸乙基五胺、二乙基胺基丙基胺等(聚)伸烷基聚胺等)、脂環族胺系硬化劑(例如：薄荷烷二胺、異佛爾酮二胺、雙(4-胺基-3-甲基環己基)甲烷、3,9-雙(3-胺基丙基)-2,4,8,10-四氧雜螺[5.5]十一烷等單環式脂肪族聚胺；降烷二胺等橋接環式聚胺等)、咪唑系硬化劑[咪唑類(例如：2-甲基咪唑、2-十七烷基咪唑、2-乙基-4-甲基咪唑等烷基咪唑；2-苯基咪唑、2-苯基-4-甲基咪唑、2-苯基-4-甲基-5-羥甲基咪唑、1-苄基-2-苯基咪唑等芳基咪唑)、咪唑類之鹽(例如：甲酸鹽、苯酚鹽、苯酚酚醛清漆鹽等有機鹽；碳酸鹽等鹽)、環氧化合物(例如雙酚A之二縮水甘油醚等聚環氧化合物)與咪唑類之反應物(或加成物)等]、酚樹脂系硬化劑(例如上述酚醛清漆型環氧樹脂之項所例示之酚醛清漆樹脂等)、酸酐系硬化劑(例如：十二烯基琥珀酸酐、己二酸酐等脂肪族羧酸酐；四氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、六氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐、甲基雙環庚烯二甲酸酐、甲基環己烯二羧酸酐等脂環族羧酸酐；鄰苯二甲酸酐、偏苯三甲酸酐、均苯四甲酸二酐、二苯甲酮四羧酸酐等芳香族羧酸酐)、聚胺基醯胺系硬化劑、聚硫醇系硬化劑、潛伏性硬化劑(三氟化硼-胺錯合物、雙氰胺、羧酸醯肼等)等。該等之硬化劑可單獨使用或將2種以上組合。再者，亦存在硬化劑作為硬化促進劑起作用之情況。
再者，芳香族胺系硬化劑與其他硬化劑之比率可自前者/後者(重量比)=100/0~30/70左右之範圍進行選擇，可為99.5/0.5~40/60(例如99/1~50/50)，較佳為98/2~70/30(例如97/3~80/20)左右。
又，關於硬化劑(或芳香族胺系硬化劑)之比率，相對於環氧樹脂100重量份，例如可為1~200重量份，較佳為2~150重量份，進而較佳為3~100重量份左右，通常可為5~80重量份(例如10~60重量份)左右。
再者，相對於環氧樹脂之環氧基1當量，硬化劑之官能基(胺基等)之比率例如可為0.1~4.0當量，較佳為0.3~2.0當量，進而較佳為0.5~1.5當量左右。
環氧樹脂組合物可包含硬化促進劑。作為硬化促進劑，可列舉慣用之硬化促進劑，例如：膦類(例如乙基膦、丙基膦、苯基膦、三苯基膦、三烷基膦等)、胺類[例如哌啶、三乙胺、二甲苄胺、三乙醇胺、二甲胺基乙醇、三乙二胺、三(二甲胺基甲基)苯酚、N,N-二甲基哌等二~三級胺類或其鹽等]等。再者，上述例示之硬化劑(例如咪唑類等)亦存在作為硬化促進劑發揮功能之情況。硬化促進劑可單獨使用或將2種以上組合使用。
關於硬化促進劑之比率，例如相對於環氧樹脂100重量份，可為0.01~50重量份，較佳為0.1~30重量份左右，通常可為0.5~30重量份(例如1~25重量份)左右。
關於具有芳香族胺骨架之樹脂成分(例如環氧樹脂組合物等)之比率，相對於金屬薄片100重量份，例如可為1~50重量份(例如2~40重量份)，較佳為3~30重量份(例如4~25重量份)，進而較佳為5~20重量份(例如5~15重量份)左右，通常可為3~15重量份(例如5~10重量份)左右。本發明中，藉由將金屬薄片與特定之樹脂成分加以組合，即便樹脂成分之比率較大，亦可提昇導電性或密接性。
(其他成分)
若有必要，可於本發明之導電性組合物中添加慣用之添加劑，例如：著色劑(染顏料等)、色相改良劑、染料定著劑、防金屬腐蝕劑、穩定劑(抗氧化劑、紫外線吸收劑等)、界面活性劑或分散劑、分散穩定劑、增黏劑或黏度調整劑、搖變性賦予劑、調平劑或光澤賦予劑、保濕劑、消泡劑、殺菌劑、填充劑等。該等添加劑可單獨使用或將兩種以上組合使用。
又，本發明之導電性組合物可包含溶劑(或分散介質)。此種組合物(特別是膏狀組合物)適合於用作塗佈用組合物(塗佈用導電性組合物)。作為溶劑，例如可列舉：醇類[例如：乙醇、丙醇、異丙醇、丁醇、2-乙基-1-己醇、癸醇等脂肪族醇；環烷醇類(環己醇等)、松脂醇、二氫松脂醇等萜烯醇類等脂環族醇；苄醇等芳香脂肪族醇；多元醇類(乙二醇、丙二醇、二乙二醇、二丙二醇等(聚)烷烴多元醇等)]、二醇醚類(例如：乙二醇單甲醚(甲基溶纖素)、乙基溶纖素、丁基溶纖素等溶纖素類；二乙二醇單甲醚(甲基卡必醇)、乙基卡必醇、丙基卡必醇、丁基卡必醇等卡必醇類；三乙二醇單甲醚、三乙二醇單乙醚、三乙二醇單丁醚、四乙二醇單丁醚等聚乙二醇單C1-6烷基醚等)、二醇醚酯類(例如溶纖素乙酸酯類、卡必醇乙酸酯類等)、烴類[例如：脂肪族烴類(例如己烷、辛烷等)、脂環式烴類(環己烷等)、鹵化烴類(二氯甲烷、氯仿、二氯乙烷等)、芳香族烴類(例如甲苯、二甲苯等)等]、酯類(例如乙酸甲酯、乙酸乙酯等)、醯胺類(N,N-二甲基甲醯胺、N,N-二甲基乙醯胺等)、酮類(丙酮、甲基乙基酮、甲基異丁基酮等)、醚類(二乙醚、二丙醚、二烷、四氫呋喃等)等。該等溶劑可單獨使用或將2種以上組合。
再者，於包含溶劑之導電性組合物(或導電膏)中，固形分濃度例如可自10~99重量%左右之範圍進行選擇，例如為20~95重量%，較佳為30~90重量%(例如50~90重量%)，進而較佳為60~85重量%，通常可為50~90重量%(例如60~80重量%)左右。
又，關於本發明之導電性組合物(特別是包含溶劑之導電性組合物)之黏度，例如於25℃下可為1~500Pa‧s(例如3~300Pa‧s)，較佳為5~250Pa‧s(例如7~200Pa‧s)，進而較佳為10~150Pa‧s左右。若黏度過小，則於塗佈(例如，點膠塗佈)時有液滴落之虞，若黏度過大，則有產生拉絲之虞。
再者，本發明之導電性組合物可藉由將各成分進行混合而製備，例如可藉由使金屬薄片分散於包含樹脂成分及(進而視需要與其他成分)溶劑(或分散介質)之系統中而製備。
[導電性組合物之用途及成形體]
本發明之導電性組合物(或導電膏)於形成需要導電性(或導電性部位)之各種成形體(導電性成形體)時有用。例如，本發明之導電性組合物可用作用以於基材上形成配線或電路(導電通路或電極)之組合物。特別是本發明之導電性組合物可實現較高之導電性或熱傳導性並且對基材之密接性或接著性優異，故而適合用作導電性接著劑。
即，導電性成形體至少具有由本發明之導電性組合物所形成之導電性部位(或導電膜)。更具體而言，於配線或電路用途中，導電性成形體可於基材上將由導電性組合物所形成之導電性部位用作配線或電路(或電極)。又，於導電性接著劑用途中，導電性成形體具備包含2片基材、及介存於該基材間且使2片基材接著(直接接著)之導電性接著劑之接合基材(接合構件)，上述導電性接著劑藉由導電性組合物而形成。
此種成形體可藉由於基材上塗佈(或塗覆(coating))導電性組合物，並進行固化或硬化處理而獲得。再者，導電性組合物通常可於形成於基材之接著層上形成，亦可不形成其他接著層等而直接塗佈於基材上。
基材(或基板)可利用無機材料(無機原材料)及/或有機材料(有機原材料)形成。作為無機材料，例如可列舉：玻璃類(鈉玻璃、硼矽酸玻璃、冕玻璃、含鋇玻璃、含鍶玻璃、含硼玻璃、低鹼玻璃、無鹼玻璃、結晶化透明玻璃、二氧化矽玻璃、石英玻璃、耐熱玻璃等)、陶瓷、金屬(鋁、銅、金、銀等)、半導體(例如以導體、半導體、絕緣體等形成之半導體等)。作為陶瓷，例如可例示：金屬氧化物(氧化矽、 石英、氧化鋁(alumina)或氧化鋁、氧化鋯、藍寶石、鐵氧體、二氧化鈦或氧化鈦、氧化鋅、氧化鋸、莫來石、氧化鈹等)、金屬氮化物(氮化鋁、氮化矽、氮化硼、氮化碳、氮化鈦等)、金屬碳化物(碳化矽、碳化硼、碳化鈦、碳化鎢等)、金屬硼化物(硼化鈦、硼化鋯等)、金屬複氧化物[鈦酸金屬鹽(鈦酸鋇、鈦酸鍶、鈦酸鉛、鈦酸鈮、鈦酸鈣、鈦酸鎂等)、鋯酸金屬鹽(鋯酸鋇、鋯酸鈣、鋯酸鉛等)等]。
作為有機材料，例如可列舉：聚甲基丙烯酸甲酯系樹脂、苯乙烯系樹脂、氯乙烯系樹脂、聚酯系樹脂[包含聚伸烷基芳酯系樹脂(聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸乙二酯等均聚或共聚伸烷基芳酯等)、聚芳酯系樹脂或液晶聚合物]、聚醯胺系樹脂、聚碳酸酯系樹脂、聚碸系樹脂、聚醚碸系樹脂、聚醯亞胺系樹脂、纖維素衍生物、氟樹脂等。
該等材料之中，較佳為耐熱性較高之材料，例如：半導體、玻璃、金屬等無機材料；工程塑膠[例如：芳香族聚酯系樹脂(聚萘二甲酸乙二酯等聚伸烷基芳酯系樹脂、聚芳酯系樹脂等)、聚醯亞胺系樹脂、聚碸系樹脂等]、液晶聚合物、氟樹脂等塑膠。
再者，以導電性組合物所構成之導電性接著劑可將相同或不同之2片基材接著。例如，可將金屬基材與金屬基材接著，亦可將金屬基材與半導體之基材接著。再者，於金屬彼此之接著中，可使非金屬之基材(例如半導體、塑膠等)上所形成之金屬或陶瓷膜(藉由蒸鍍等之金屬膜、金屬氧化物膜等)接著。作為更具體之例，例如於半導體領域中，可利用導電性接著劑(黏晶膏)使作為一基材之引線框架[例如：以金屬(銅、銅合金、鋁等)所形成之引線框架、由金屬形成且進而經鍍敷處理之引線框架等]、與作為另一基材之半導體基板(或半導體晶片)[例如：半導體基材(矽基板等)、於半導體基材(矽基板等)上形成有金屬膜(鈦、鉑、金等)、電路、電極等導電膜(ITO膜等)之半導體晶 片等]接著。
可對基材之表面實施氧化處理[表面氧化處理，例如：放電處理(電暈放電處理、輝光放電等)、酸處理(鉻酸處理等)、紫外線照射處理、火焰處理等]、表面凹凸處理(溶劑處理、噴砂處理等)等表面處理。
基材之厚度可根據用途進行選擇，例如可為0.001~10mm，較佳為0.01~5mm，進而較佳為0.05~3mm左右。
作為對基材之導電性組合物之塗佈方法，例如可例示：流塗法、旋轉塗佈法、噴塗法、塗鑄法、棒式塗佈法、簾幕式塗佈法、輥塗法、浸漬法、狹縫法、光微影法、各種印刷法(網版印刷法、軟版印刷法、凹版塗佈法、噴墨法)等。導電性組合物可根據用途應用於基材整個面的至少一部分(一部分或全部)。例如，於形成配線或電路之情形時，可藉由導電性組合物形成圖案狀之塗膜，於用作導電性接著劑之情形時，可使之對應於2片基材間之被接著部位而形成導電性組合物之塗膜。再者，於將塗膜形成為圖案狀之情形時，例如可利用網版印刷法、噴墨印刷法、凹版印刷法(例如，凹版印刷法等)、套版印刷法、凹版套版印刷法、軟版印刷法等進行塗佈。
塗佈後可自然乾燥或進行加熱而乾燥。加熱溫度可根據溶劑之種類進行選擇，例如為50~200℃，較佳為80~180℃，進而較佳為100~150℃(特別是110~140℃)左右。加熱時間例如為1分鐘~3小時，較佳為5分鐘~2小時，進而較佳為10分鐘~1小時左右。
未硬化(前驅物)狀態之塗膜通常被供於硬化處理。硬化處理通常可藉由至少進行加熱(或燒成或加熱處理)而進行。加熱溫度(熱處理溫度)例如可為100~350℃，較佳為120~320℃，進而較佳為150~300℃(例如180~250℃)左右。又，加熱時間根據加熱溫度等，例如可為10分鐘~5小時，較佳為15分鐘~3小時，進而較佳為20分鐘~1小時 左右。
所獲得之導電性部位或導電膜(硬化處理後之塗膜、燒結圖案)之厚度可根據用途自0.01~10000μm左右之範圍進行選擇，例如可為0.01~100μm，較佳為0.1~50μm，進而較佳為0.3~30μm(特別是0.5~10μm)左右。本發明中，可形成相對厚膜，例如0.3μm以上(例如0.3~100μm)、較佳為0.5μm以上(例如，0.5~50μm)、進而較佳為1μm以上(例如1~30μm)左右之厚度之金屬膜。即便為此種厚膜，亦可於無損對基材之密接性之情況下形成較高之導電膜。
於本發明之上述導電性成形體中，介存於基材間之導電性部位之值X可為30%以下(例如25%以下，較佳為10%以下，更佳為5%以下，特別是3%以下)。於本發明中，值X可採用在與基材接觸之側(基材側)或表面側所測定之值。再者，導電性部位之上述值X存在因測定部位(厚度方向之部位)而稍微不同之情況，即便為此種情形時，較多情形時值X亦在上述範圍內。例如，於薄膜(例如厚度200~400μm左右之薄膜)之表面側所測定之值X為10%以下，較佳為5%以下(例如0.5~3%)，更佳為3%以下(例如1~2.5%)。又，若導電性部位之厚度變大，則於導電性部位之中心部(遠離表面部之內部)，隨著配向性之降低而呈值X變大之傾向。例如，厚度5mm左右之厚膜之導電性部位(導電膜)之內部(於厚度方向之中央部附近切開之測定面)之值X可超過30%，但通常可為30%以下(例如5~27%)，較佳為25%以下(例如20~25%)左右。
[實施例]
以下，基於實施例更詳細地說明本發明，但本發明並不受該等實施例之限定。實施例及比較例所使用之各種成分如下所述。
(芳香族胺樹脂成分A)
對雙酚A丙氧基二縮水甘油醚(和光純藥工業(股)製造，環氧當量 228g/eq)3.75重量份混合芳香族聚胺[東京化成製造，4,4'-亞甲基雙(2-乙基-6-甲基苯胺)]1.25重量份，而製作芳香族胺樹脂成分A。
(芳香族胺樹脂成分B)
對雙酚A丙氧基二縮水甘油醚(和光純藥工業(股份)製造，環氧當量228g/eq)3.73重量份混合芳香族聚胺(和光純藥工業(股份)製造，4,4'-二胺基二苯醚)1.27重量份，而製作芳香族胺樹脂成分B。
(芳香族胺樹脂成分C)
對苯酚酚醛清漆型環氧樹脂(三菱化學製造，「jER152」，環氧當量174g/eq)3.56重量份混合芳香族聚胺[東京化成製造，4,4'-亞甲基雙(2-乙基-6-甲基苯胺)]1.44重量份，而製作芳香族胺樹脂成分C。
(非芳香族胺樹脂成分A)
對雙酚A丙氧基二縮水甘油醚(和光純藥工業(股份)製造，環氧當量228g/eq)4.75重量份混合雙氰胺(三菱化學製造，「DICY-7」)0.25重量份，而製作非芳香族胺樹脂成分A。
(非芳香族胺樹脂成分B)
對雙酚A丙氧基二縮水甘油醚(和光純藥工業(股份)製造，環氧當量228g/eq)4.17重量份混合咪唑類(咪唑系環氧加成物硬化劑，Ajinomoto Fine-Techno製造，PN-23)0.83重量份，而製作非芳香族胺樹脂成分B。
(非芳香族胺樹脂成分C)
對雙酚A丙氧基二縮水甘油醚(和光純藥工業(股份)製造，環氧當量228g/eq)2.84重量份混合甲基-1,2,3,6-四氫鄰苯二甲酸酐(和光純藥工業(股份)製造)2.07重量份、及二甲苄胺0.01重量份，而製作非芳香族胺樹脂成分C。
(銀薄片A)
依據日本專利第4144856號公報之實施例2，而製作銀薄片A。所 獲得之銀薄片A之平均粒徑(D50)為6.2μm，值X為5.01%。
(銀薄片B)
依據日本專利第4399799號公報之實施例2，而製作銀薄片B。所獲得之銀薄片A之平均粒徑(D50)為2.2μm，值X為7.88%。
(銀薄片C)
使用市售之銀薄片(三井金屬礦業(股份)製造，「Q03R flakes 2」)。該銀薄片係利用球磨機將藉由銀鹽之液相還原而製備之球狀銀粉進行扁平化而成者，平均粒徑(D50)為1.1μm，值X為30.8%。
再者，以下表示各種物性、特性之測定方法或評價方法。
(平均粒徑)
銀薄片之平均粒徑(D50)係使用雷射繞射散射式粒度分佈測定裝置(日機裝製造，「Microtrac」)所測定之體積基準中心粒徑。
(結晶性)
銀薄片之結晶性如以下般進行測定。
將推壓環安裝於距試樣固持器之試樣面約低2mm之位置，並加入銀薄片粉末。使試樣面密接於玻璃板後，利用推壓治具自相反側對推壓環進行推壓，以試樣面成為平坦之方式將銀薄片粉末固定，而製作測定試樣。
使用X射線繞射裝置(RIGAKU製造，RINT1200)，測定條件以2θ/θ掃描法、X射線之波長為CuKα射線(λ=0.15418nm)、掃描角35-55°進行，將自來自銀之約38°之(111)面及約44°之(200)面之繞射波峰之積分強度值分別設為I111、I200，算出值X=[I200/(I111+I200)]×100(%)。
又，導電性組合物(或其硬化物)之結晶性以如下方式進行測定。
利用敷料器將導電性組合物塗佈於聚四氟乙烯(PTFE)板上，於120℃下加熱30分鐘，繼而於200℃下加熱90分鐘，製作厚度約200~ 400μm之薄膜狀硬化物。自聚四氟乙烯板剝離薄膜狀硬化物，針對經敷料器塗佈之面(表面側)及連接於PTFE板之面(PTFE側)，分別以與上述銀薄片相同之條件進行X射線繞射之測定，算出值X。
(比電阻)
使用敷料器將導電性組合物塗佈於載玻片，於120℃下乾燥30分鐘後，於200℃下燒成90分鐘形成厚度15μm之導電膜，根據藉由四探針法而得之表面電阻及藉由觸針式膜厚計而得之膜厚算出比電阻。
(剝離試驗)
使用敷料器將導電性組合物塗佈於載玻片(基板)，於120℃下乾燥30分鐘後，於200℃下燒成90分鐘形成厚度15μm之導電膜。
將寬度24mm之透明膠帶(Nichiban公司製造)貼附於玻璃基板上所形成之導電膜，並施加5kg重左右之荷重後，使荷重擦過以使導電膜與透明膠帶之間之氣泡消失，藉此去除氣泡而使透明膠帶與基板密接。其後，將基板固定並上拉透明膠帶，以基板與膠帶之角度成為約90度之方式一面集中精神一面以約0.6秒之速度瞬間剝離，將膠帶完全未附著導電膜之剝離之情況判定為密接性良好(○)，將導電膜之一部分或全部剝離之情況判定為密接性不良好(×)。
(接著強度)
使用導電性組合物將3.5mm×3.5mm之矽晶片貼附於厚度2mm之銅板，並於120℃下乾燥30分鐘後，於200℃下燒成90分鐘，使矽晶片與銅板接著，其後，對剪切強度進行測定，藉此進行評價。再者，矽晶片於矽上具備按鈦、鉑、金之順序進行濺鍍之蒸鍍膜，並以接著面作為金之蒸鍍面。硬化後之接著層之厚度為30μm。再者，關於接著強度，針對4個樣品進行測定。
(熱傳導率)
使用所測定之比電阻值，並使用藉由維德曼-夫蘭茲定律 (Wiedemann-Franz law)之式λ=L×T/ρv(λ為熱傳導率，L為勞倫茲(Lorentz)數(2.44×10-8W‧Ω‧K-2)，T為絕對溫度(298K)，ρv為比電阻)，而測定熱傳導率。
(實施例1)
將100重量份之銀薄片A、5重量份之芳香族胺樹脂成分A、作為溶劑之三乙二醇單丁醚(和光純藥工業(股份)製造)10重量份利用三輥磨進行混練，而獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.92%，於PTFE側為1.65%。
(實施例2)
於實施例1中使用5重量份之芳香族胺樹脂成分B代替5重量份之芳香族胺樹脂成分A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.54%，於PTFE側為1.44%。
(實施例3)
於實施例1中使用5重量份之芳香族胺樹脂成分C代替5重量份之芳香族胺樹脂成分A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.64%，於PTFE側為1.23%。
(實施例4)
於實施例1中使用7.5重量份芳香族胺樹脂成分A代替5重量份，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.13%，於PTFE側為1.04%。
(實施例5)
於實施例1中使用10重量份芳香族胺樹脂成分A代替5重量份，除 此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.28%，於PTFE側為1.23%。
(實施例6)
於實施例1中使用100重量份之銀薄片B代替100重量份之銀薄片A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為3.74%，於PTFE側為2.25%。
(比較例1)
於實施例1中使用5重量份之非芳香族胺樹脂成分A代替5重量份之芳香族胺樹脂成分A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.42%，於PTFE側為1.11%。
(比較例2)
於實施例1中使用5重量份之非芳香族胺樹脂成分B代替5重量份之芳香族胺樹脂成分A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.62%，於PTFE側為1.54%。
(比較例3)
於實施例1中使用5重量份之非芳香族胺樹脂成分C代替5重量份之芳香族胺樹脂成分A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為1.79%，於PTFE側為1.86%。
(比較例4)
於實施例1中使用100重量份之銀薄片C代替100重量份之銀薄片A，除此以外，與實施例1同樣地獲得導電性組合物。繼而，針對所 獲得之導電性組合物，對各種特性進行評價。再者，關於硬化物之值X，於表面側為30.8%，於PTFE側為30.4%。
將結果示於表1。再者，於表1中，所謂「胺型」意指「胺樹脂成分」之略稱。
於表1中，使用結晶性較大之(值X較小)銀薄片及芳香族胺樹脂成分之實施例1~6中，除獲得較高之導電性(較小之比電阻)、及較高之放熱性(較大之熱傳導率)以外，對基材之密接性(剝離試驗、剪切強度)亦較高。相對於此，即便使用結晶性較大之(值X較小)銀薄片，樹脂成分為非芳香族胺型之比較例1~3中，亦變得導電性較小(比電阻較大)，放熱性亦較小(熱傳導率較小)、對基材之密接性亦稍微小。又，即便使用芳香族胺樹脂成分，銀薄片之結晶性較小之(值X較大)比較例4中，亦變得導電性較小(比電阻較大)，放熱性亦較小(熱傳導率較小)，對基材之密接性亦稍微小。
再者，如以下般對上述實施例及比較例之導電性組合物之厚膜內部之值X進行測定。將導電性組合物注入至成形模(深度5mm，直徑10mmΦ)進行成形，取下成形模之後，於120℃下加熱30分鐘，繼 而於200℃下加熱90分鐘，而製作厚膜硬化物。將該試樣於厚度方向之中央部切開，針對切斷面測定值X。將結果示於表2。
根據表2，使用結晶性金屬薄片之實施例1~6及比較例1~3中，厚膜內部之值X為22~25%，與薄膜之表面部相比變大。另一方面，使用結晶性較小之金屬薄片之比較例4中，顯示出與薄膜之表面部同等之值X，為35%較大。
[產業上之可利用性]
本發明之導電性組合物由於可實現較高之導電性，故而可用作各種用途，例如用以形成配線、電路、電極等之組合物、或導電性接著劑等。特別是由於可於無損較高之密接性之情況下實現較高之導電性或放熱性，故而適合作為將2片基材間接著之導電性接著劑。
詳細且參照特定之實施態樣對本發明進行了說明，但對於業者而言，明確可於不脫離本發明之精神及範圍之情況下加以各種變更或修正。
本申請案係基於2014年2月24日提出申請之日本專利申請案2014-032895及2015年2月5日提出申請之日本專利申請案2015-021464者， 其內容作為參照而被引入本文中。

Claims (12)

  1. 一種導電性組合物，其係包含導電性金屬粉及樹脂成分之組合物，且導電性金屬粉至少包含具有金屬結晶成長為薄片狀之晶體結構之金屬薄片，上述樹脂成分包含芳香族胺骨架。
  2. 如請求項1之導電性組合物，其中於將X射線繞射之(111)面、(200)面之繞射積分強度分別設為I111、I200時，金屬薄片為下述式所表示之值X為30%以下之金屬薄片；X=[I200/(I111+I200)]×100(%)。
  3. 如請求項1之導電性組合物，其中樹脂成分為包含熱硬化性樹脂及硬化劑之熱硬化性樹脂組合物，熱硬化性樹脂及/或硬化劑包含芳香族胺骨架。
  4. 如請求項3之導電性組合物，其中熱硬化性樹脂為環氧樹脂，硬化劑為芳香族胺系硬化劑。
  5. 如請求項3之導電性組合物，其中硬化劑為具有芳香環上直接取代有胺基之結構之芳香族胺系硬化劑。
  6. 如請求項3之導電性組合物，其中硬化劑包含下述式(1)所表示之芳香族聚胺； (式中，環Z分別獨立，表示芳烴環，A表示伸烷基或亞烷基、伸環烷基或亞環烷基、伸芳基、氧原子、硫原子、亞磺醯基、或磺醯基，R表示烷基、環烷基、芳基、芳烷基、烷氧基、或鹵 素原子，m表示0或1，n分別獨立表示0~4之整數)。
  7. 如請求項1之導電性組合物，其中樹脂成分之比率相對於金屬薄片100重量份為1~50重量份。
  8. 如請求項1之導電性組合物，其係導電性接著劑。
  9. 如請求項1之導電性組合物，其係用以使金屬基材與半導體基材接著之導電性接著劑。
  10. 一種導電性成形體，其至少具有由如請求項1至9中任一項之導電性組合物所形成之導電性部位。
  11. 如請求項10之導電性成形體，其係具備由2片基材、及介存於該基材間且使2片基材接著之導電性接著劑所構成之接合基材之成形體，且作為導電性部位之導電性接著劑係由如請求項1至9中任一項之導電性組合物而形成。
  12. 如請求項10或11之導電性成形體，其中於將X射線繞射之(111)面、(200)面之繞射積分強度分別設為I111、I200時，下述式所表示之值X於導電性部位為30%以下；X=[I200/(I111+I200)]×100(%)。
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