TWI556260B - Conductive particles, anisotropic conductive materials and connecting structures - Google Patents

Conductive particles, anisotropic conductive materials and connecting structures Download PDF

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Publication number
TWI556260B
TWI556260B TW100135338A TW100135338A TWI556260B TW I556260 B TWI556260 B TW I556260B TW 100135338 A TW100135338 A TW 100135338A TW 100135338 A TW100135338 A TW 100135338A TW I556260 B TWI556260 B TW I556260B
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Taiwan
Prior art keywords
copper
particles
tin
conductive
layer
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TW100135338A
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English (en)
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TW201222558A (en
Inventor
Xiaoge Wang
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Sekisui Chemical Co Ltd
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Publication of TW201222558A publication Critical patent/TW201222558A/zh
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
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Description

導電性粒子、異向性導電材料及連接構造體
本發明，例如，係關於一種可用於電極間之連接之導電性粒子，更為詳細而言係關於一種具有基材粒子及設置於該基材粒子之表面上之導電層之導電性粒子。又，本發明係關於使用上述導電性粒子之異向性導電材料及連接構造體。
異向性導電膏及異向性導電膜等異向性導電材料已廣為人知。該等異向性導電材料係於黏合樹脂中分散有導電性粒子。
上述異向性導電材料可用於IC(Integrated Circuit，積體電路)晶片與可撓性印刷電路基板之連接、及IC晶片與具有ITO(Indium-Tin Oxide，氧化銦錫)電極之電路基板的連接等。例如，於將異向性導電材料配置於IC晶片之電極與電路基板之電極之間後，進行加熱及加壓，藉此可將該等電極電性連接。
作為上述異向性導電材料所使用之導電性粒子之一例，於下述專利文獻1中揭示有具備樹脂粒子、及設置於該樹脂粒子之表面上之銅層的導電性粒子。於專利文獻1中，並未以具體之實施例揭示此種導電性粒子，但記載有可於相對向之電路之連接中獲得良好之電性連接。
如較多地用於專利文獻1所記載之實施例中般，先前具有鎳層之導電性粒子為主流。然而，鎳本身存在電阻較高、難以降低連接電阻之問題。相對於此，銅由於電阻較低，故就降低連接電阻之觀點而言，若將銅用作導電性粒子之導電層則較為有利。然而，銅具有與鎳等相比較軟之性質。因此，由銅所形成之導電層過軟，若對於導電性粒子賦予較大之力，則易於導電層中產生裂痕。例如，於將先前之導電性粒子用於電極間之連接而獲得連接構造體之情形時，有於導電層中產生較大之裂痕之情況。因此，有無法確實地將電極間連接之情況。
又，作為具有含有銅之導電層之導電性粒子，於下述專利文獻2中揭示有具有錫-銀-銅之三元系合金覆膜的導電性粒子。於專利文獻2之實施例中，為了獲得導電性粒子，而於銅金屬粒子之表面形成鍍錫覆膜，繼而形成鍍銀覆膜，藉由加熱至240℃以上而引起金屬熱擴散，形成錫-銀-銅之三元系合金覆膜。
上述專利文獻2中記載有，錫-銀-銅三元系之合金覆膜中之組成之含有比例係錫為80~99.8重量%、銀為0.1~10重量%、銅為0.1~10重量%。具體而言，於上述專利文獻2之全部實施例中形成有錫為96.5重量%、銀為3重量%、銅為0.5重量%之合金覆膜。該導電性粒子含有相對較少之銀及銅且含有相對較多之錫，故而錫-銀-銅之三元系合金覆膜之熔點變得相對較低。含有具有熔點較低之導電層之導電性粒子的異向性導電材料於為形成連接構造體而進行熱壓接時，由於存在由熱引起導電層之流動且流出必要以上之情況，進而由於與電極連接之導電層之厚度變得過薄，故而存在產生連接不良之情況。
[先前技術文獻] [專利文獻]
[專利文獻1]日本專利特開2003-323813號公報
[專利文獻2]WO2006/080289A1
本發明之目的在於提供一種即便對導電性粒子賦予較大之力亦難以於導電層中產生較大之裂痕的導電性粒子、以及使用該導電性粒子之異向性導電材料及連接構造體。
又，本發明之限定性之目的在於提供一種銅-錫層之熔點較高且於為形成連接構造體而進行熱壓接時可抑制銅-錫層之過度之熱變形及流出的導電性粒子，以及使用該導電性粒子之異向性導電材料及連接構造體。
根據本發明之廣泛態樣，提供一種導電性粒子，其具備基材粒子及設置於該基材粒子之表面上之含有銅與錫之銅-錫層，且該銅-錫層含有銅與錫之合金，該銅-錫層整體中之銅之含量超過20重量%且為75重量%以下，並且錫之含量為25重量%以上且未達80重量%。
於本發明之導電性粒子之某一特定態樣中，上述銅-錫層之熔點為550℃以上。
於本發明之導電性粒子之某一特定態樣中，上述銅-錫層整體中之銅之含量為40重量%以上、60重量%以下，且錫之含量為40重量%以上、60重量%以下。
於本發明之導電性粒子之某一特定態樣中，該導電性粒子於表面上具有突起。
於本發明之導電性粒子之另一特定態樣中，具備配置於上述銅-錫層之表面上之絕緣性物質。
於本發明之導電性粒子之進而另一特定態樣中，上述絕緣性物質為絕緣性粒子。
本發明之異向性導電材料含有依據本發明所構成之導電性粒子及黏合樹脂。
本發明之連接構造體具備第1連接對象構件、第2連接對象構件、及連接該第1、第2連接對象構件之連接部，且該連接部係藉由依據本發明所構成之導電性粒子而形成，或藉由含有該導電性粒子及黏合樹脂之異向性導電材料而形成。
本發明之導電性粒子由於在基材粒子之表面上設置有含有銅與錫之銅-錫層，該銅-錫層含有銅與錫之合金，進而該銅-錫層整體中之銅之含量超過20重量%且為75重量%以下，並且錫之含量為25重量%以上且未達80重量%，故而即便對導電性粒子賦予較大之力亦難以於導電層中產生較大之裂痕。
以下，藉由一面參照圖式一面對本發明之具體實施形態及實施例進行說明而明確本發明。
圖1係表示本發明之第1實施形態之導電性粒子的剖面圖。
圖1所示之導電性粒子1具備基材粒子2、及設置於該基材粒子2之表面2a上之銅-錫層3。銅-錫層3為導電層(第1導電層)。導電性粒子1亦可進而具備配置於銅-錫層3之表面3a上之絕緣性物質。進而，亦可於銅-錫層3之表面3a上積層鈀層等其他導電層(第2導電層)。上述絕緣性物質亦可經由鈀層等其他導電層而間接地配置於銅-錫層3之表面3a上。
銅-錫層3含有銅與錫之合金。於本實施形態中，銅-錫層3為銅-錫合金層。銅-錫層之一部分區域亦可不含錫，銅-錫層之一部分區域亦可不含銅。例如，銅-錫層之內側部分亦可僅含銅，銅-錫層之外側部分亦可僅含錫。銅-錫層3整體中之銅之含量超過20重量%且為75重量%以下，並且錫之含量為25重量%以上且未達80重量%。
本實施形態之特徵在於：設置於基材粒子2之表面2a上之銅-錫層3含有銅與錫之合金，且銅-錫層3整體中之銅之含量超過20重量%且為75重量%以下，並且錫之含量為25重量%以上且未達80重量%。藉由形成此種銅-錫層3，即便對導電層賦予較大之力亦難以於導電層中產生較大之裂痕。可認為其原因在於：藉由銅與錫之合金化，銅-錫層3之硬度適度地變高。因此，於將導電性粒子1用於電極間之連接而獲得連接構造體之情形時，難以於導電層中產生較大之裂痕，且可提高電極間之導通可靠性。再者，所謂上述較大之裂痕，係指導電層自基材粒子剝離並脫落而產生電極間之連接不良之程度的裂痕。進而，銅-錫層3由於含有相對較多之銅，故而可降低電極間之連接電阻。
再者，銅與鎳相比導通性較高。因此，為了提高導通性，較佳為使用銅而並非鎳。本發明係於導電層中使用銅。又，本發明與通常稱為焊錫之導電物質不同，使用相對較多之銅。
銅-錫層3整體中之銅之含量較佳為30重量%以上、更佳為35重量%以上、進而較佳為40重量%以上，較佳為70重量%以下。銅-錫層3整體中之錫之含量較佳為30重量%以上，較佳為70重量%以下、更佳為65重量%以下、進而較佳為60重量%以下。
較佳為，銅-錫層3整體中之銅之含量為30重量%以上、70重量%以下，且錫之含量為30重量%以上、70重量%以下。更佳為，銅-錫層3整體中之銅之含量為35重量%以上、65重量%以下，且錫之含量為35重量%以上、65重量%以下。進而較佳為，銅-錫層3整體中之銅之含量為40重量%以上、60重量%以下，且錫之含量為40重量%以上、60重量%以下。
尤其是，於銅-錫層3整體中之銅之含量為40重量%以上、60重量%以下，且錫之含量為40重量%以上、60重量%以下之情形時，即便對導電層賦予較大之力，亦更難以於導電層中產生較大之裂痕。
再者，本發明中之銅與錫等金屬之各含量係以重量%表示銅或錫相對於導電層之金屬之總重量的分量而獲得之值。作為其測定方法，可列舉如下者：以王水溶化導電層之金屬，使用ICP((Inductively Coupled Plasma)電感耦合電漿，堀場製作所製造之「ULTIMA2」)測量溶解有該金屬之溶液，根據所獲得之金屬離子濃度計算導電層之金屬之重量及各金屬之分量。
圖1所示之導電性粒子1例如可使用圖4所示之導電性粒子而獲得。
於基材粒子2之表面2a上形成含有銅之銅層52。繼而，於銅層52之表面52a上形成含有錫之錫層53，獲得加熱前之導電性粒子51。繼而，加熱導電性粒子51使銅與錫合金化。為了使銅與錫高效地合金化，上述加熱之溫度較佳為150℃以上、更佳為180℃以上，較佳為250℃以下、更佳為230℃以下。為了使銅與錫高效地合金化，尤佳為於200~220℃下將導電性粒子加熱18~24小時。銅-錫層3較佳為以含有銅與錫之合金之方式於150℃以上進行加熱處理之銅-錫層。
於導電性粒子51中，可藉由調整銅層52與錫層53之各厚度而調整銅-錫層3整體中之銅之含量及錫之含量。
本發明之導電性粒子較佳為藉由對在基材粒子之表面上設置有銅層且於該銅層之表面上設置有錫層的導電性粒子進行加熱而獲得之導電性粒子。
圖2係表示本發明之第2實施形態之導電性粒子的剖面圖。
圖2所示之導電性粒子11具備基材粒子2、及設置於該基材粒子2之表面2a上之銅-錫層12。銅-錫層12為導電層。導電性粒子11於基材粒子2之表面2a上具備複數個芯物質13。作為導電層之銅-錫層12被覆芯物質13。導電層被覆芯物質13，藉此導電性粒子11於表面11a上具有複數個突起14。導電性粒子11於銅-錫層12外側之表面12a上具有複數個突起14。突起14係形成於銅-錫層12之表面12a上。銅-錫層12之表面12a因芯物質13而隆起，從而形成突起14。於突起14之內側配置有芯物質13。於銅-錫層12之表面12a上亦可積層有鈀層等其他導電層。
導電性粒子11具備配置於銅-錫層12之表面12a上之絕緣性粒子15。絕緣性粒子15為絕緣性物質。於銅-錫層與絕緣性粒子間亦可存在鈀層等其他導電層。於本實施形態中，銅-錫層12之表面12a之一部分區域藉由絕緣性粒子15而被覆。如此，導電性粒子亦可具備附著於銅-錫層等導電層之表面上之絕緣性粒子15。但是，亦可不必具備絕緣性粒子15。進而，除絕緣性粒子15以外亦可具備絕緣性樹脂層。導電性粒子亦可具備附著於銅-錫層等導電層之表面上之絕緣性樹脂層。銅-錫層等導電層之表面亦可藉由絕緣性樹脂層而被覆。該絕緣性樹脂層為絕緣性物質。
於圖5中，以剖面圖表示本發明之第3實施形態之導電性粒子。
圖5所示之導電性粒子61具備基材粒子2、銅-錫層3、及第2導電層62。第2導電層62係設置於導電性粒子1中之銅-錫層3之表面3a上。第2導電層62與銅-錫層3不同。又，亦可於導電性粒子11中之銅-錫層12之表面12a上設置第2導電層。進而，亦可於基材粒子之表面上設置第2導電層，並於該第2導電層上設置銅-錫層。即，亦可於基材粒子與銅-錫層間配置第2導電層。
圖6中，以剖面圖表示本發明之第4實施形態之導電性粒子。
圖6中所示之導電性粒子71具備基材粒子2、及設置於該基材粒子2之表面2a上之銅-錫層72。銅-錫層72具有第1區域、及厚度較第1區域薄之區域。銅-錫層72具有厚度不均。
作為上述基材粒子，可列舉樹脂粒子、無機粒子、有機無機混合粒子及金屬粒子等。
上述基材粒子較佳為由樹脂所形成之樹脂粒子。於連接電極間時，將導電性粒子配置於電極間後，通常使導電性粒子壓縮。若基材粒子為樹脂粒子，則導電性粒子藉由壓縮而易變形，導電性粒子與電極之接觸面積增大。因此，可提高電極間之導通可靠性。
作為用以形成上述樹脂粒子之樹脂，可較佳地使用各種有機物。作為用以形成上述樹脂粒子之樹脂，例如可使用：聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚偏二氯乙烯、聚丙烯、聚異丁烯、聚丁二烯等聚烯烴，聚甲基丙烯酸甲酯、聚丙烯酸甲酯等丙烯酸系樹脂，聚對苯二甲酸伸烷基酯，聚碸，聚碳酸酯，聚醯胺，苯酚甲醛樹脂，三聚氰胺甲醛樹脂，苯并胍胺甲醛樹脂，脲甲醛樹脂等。例如，藉由使1種或2種以上之具有乙烯性不飽和基之各種聚合性單體聚合，可設計及合成具有適於導電材料之任意壓縮時之物性的樹脂粒子。
於使具有乙烯性不飽和基之單體聚合而獲得上述樹脂粒子之情形時，作為該具有乙烯性不飽和基之單體，可列舉非交聯性單體及交聯性單體。
作為上述非交聯性單體，例如可列舉：苯乙烯、α-甲基苯乙烯等苯乙烯系單體，(甲基)丙烯酸、順丁烯二酸、順丁烯二酸酐等含羧基之單體，(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸十六烷基酯、(甲基)丙烯酸硬脂基酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸異基酯等(甲基)丙烯酸烷基酯類，(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸甘油酯、聚氧乙烯(甲基)丙烯酸酯、(甲基)丙烯酸縮水甘油酯等含氧原子之(甲基)丙烯酸酯類，(甲基)丙烯腈等含腈之單體，甲基乙烯基醚、乙基乙烯基醚、丙基乙烯基醚等乙烯基醚類，乙酸乙烯酯、丁酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯等酸乙烯酯類，乙烯、丙烯、異戊二烯、丁二烯等不飽和烴，(甲基)丙烯酸三氟甲酯、(甲基)丙烯酸五氟乙酯、氯乙烯、氟乙烯、氯苯乙烯等含鹵素之單體等。
作為上述交聯性單體，例如可列舉：四羥甲基甲烷四(甲基)丙烯酸酯、四羥甲基甲烷三(甲基)丙烯酸酯、四羥甲基甲烷二(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、三(甲基)丙烯酸甘油酯、二(甲基)丙烯酸甘油酯、(聚)乙二醇二(甲基)丙烯酸酯、(聚)丙二醇二(甲基)丙烯酸酯、(聚)二(甲基)丙烯酸四亞甲基酯、1,4-丁二醇二(甲基)丙烯酸酯等多官能(甲基)丙烯酸酯類，(異)氰尿酸三烯丙酯、偏苯三甲酸三烯丙酯、二乙烯基苯、鄰苯二甲酸二烯丙酯、二烯丙基丙烯醯胺、二烯丙基醚、γ-(甲基)丙烯醯氧基丙基三甲氧基矽烷、三甲氧基矽烷基苯乙烯、乙烯基三甲氧基矽烷等含矽烷之單體等。
可藉由利用公知之方法使上述具有乙烯性不飽和基之聚合性單體聚合而獲得上述樹脂粒子。作為此方法，例如可列舉：於自由基聚合起始劑之存在下進行懸浮聚合之方法，及使單體與自由基聚合起始劑一起膨潤而使非交聯之種粒子聚合之方法等。
於上述基材粒子為無機粒子或有機無機混合粒子之情形時，作為用以形成基材粒子之無機物，可列舉二氧化矽及碳黑等。作為由上述二氧化矽所形成之粒子並無特別限定，例如可列舉使具有2個以上之水解性烷氧基之矽化合物水解而形成交聯聚合物粒子後，藉由視需要進行焙燒而獲得之粒子。
於上述基材粒子為金屬粒子之情形時，作為用以形成該金屬粒子之金屬，可列舉銀、銅、鎳、矽、金及鈦等。但是，較佳為基材粒子並非金屬粒子。
上述基材粒子之平均粒徑較佳為1~100 μm之範圍內。若基材粒子之平均粒徑為1 μm以上，則可進一步提高電極間之導通可靠性。若基材粒子之平均粒徑為100 μm以下，則可使電極間之間隔變窄。基材粒子之平均粒徑之更佳之下限為2 μm，更佳之上限為50 μm、進而較佳之上限為30 μm、尤佳之上限為5 μm。
上述平均粒徑表示數量平均粒徑。該平均粒徑例如可使用庫爾特計數器(Beckman Coulter公司製造)而測定。
關於上述銅-錫層，外表面可為平滑之球狀，於存在鱗片狀或板狀金屬小片所形成之凹凸之形態下，外表面亦可為大致球狀。又，上述銅-錫層可為單層之導電層，亦可為積層有複數層鱗片狀或板狀導電性物質之導電層。
上述銅-錫層之維氏硬度(Hv)較佳為100以上，較佳為500以下。若上述銅-錫層之維氏硬度為上述下限以上及上述上限以下，則更難以產生導電層之裂痕，且連接構造體中之導通可靠性進一步提高。
上述銅-錫層之熔點較佳為550℃以上，更佳為600℃以上。上述銅-錫層之熔點之上限並無特別限定。若上述銅-錫層之熔點為上述下限以上，則可抑制銅-錫層之過度之熱變形及流出。
上述銅-錫層之熔點係利用DSC(示差掃描熱量測定，SII公司製造「EXSTAR X-DSC7000」)而測得之值。
上述銅-錫層亦可具有第1區域、及厚度較第1區域薄之第2區域。上述銅-錫層中之最大厚度可超過最小厚度之1倍，亦可為1.1倍以上，亦可為1.5倍以上，亦可為2倍以上。若上述銅-錫層之厚度不均較大，則於使用含有導電性粒子及黏合樹脂之異向性導電材料而獲得連接構造體時，有效地去除導電性粒子與電極間之黏合樹脂。因此，所獲得之連接構造體中之導通可靠性提高。再者，藉由利用下述物理性或機械性混成法形成上述銅-錫層而容易使厚度不均變大。
上述銅-錫層之平均厚度較佳為10~1000 nm之範圍內。銅-錫層之平均厚度之更佳之下限為20 nm、進而較佳之下限為50 nm，更佳之上限為800 nm、進而較佳之上限為500 nm、尤佳之上限為300 nm。若銅-錫層之平均厚度為上述下限以上，則可進一步提高導電性粒子之導電性。若銅-錫層之平均厚度為上述上限以下，則基材粒子與銅-錫層之熱膨脹係數之差減小，銅-錫層難以自基材粒子剝離。
作為為了形成上述銅-錫層而於基材粒子之表面上形成銅層之方法，可列舉：藉由非電解鍍敷而形成銅層之方法、以及藉由電鍍而形成銅層之方法等。作為為了形成銅-錫層而於例如銅層之表面上形成錫層之方法，可列舉：藉由非電解鍍敷而形成錫層之方法、以及藉由電鍍而形成錫層之方法等。又，作為形成上述銅-錫層之較佳之方法，可使用物理性或機械性之形成方法，亦可使用物理性或機械性混成法。於物理性或機械性混成法中，可使用混合器等。
於不阻礙本發明之目的之範圍內，上述銅-錫層可含有除銅與錫以外之其他金屬。作為上述其他金屬，例如可列舉：金、銀、鈀、鉑、鈀、鋅、鐵、鉛、鋁、鈷、銦、鎳、鉻、鈦、銻、鉍、鉈、鍺、鎘、鎢、矽及摻錫氧化銦(ITO)等。
於上述銅-錫層含有上述其他金屬之情形時，銅-錫層整體中之上述其他金屬之含量較佳為20重量%以下、更佳為10重量%以下、進而較佳為5重量%以下、尤佳為1重量%以下。
上述導電性粒子亦可具有上述第2導電層。該第2導電層係與銅-錫層不同之導電層。第2導電層較佳為金層、鎳層、鈀層、銅層或含有錫與銀之合金層，更佳為鈀層或金層，進而較佳為鈀層。上述第2導電層較佳為設置於銅-錫層之表面上。
上述第2導電層之平均厚度較佳為5 nm以上。若上述第2導電層之平均厚度為5 nm以上，則容易利用上述第2導電層進行均勻之被覆。於上述第2導電層設置於上述銅-錫層之表面上之情形時，導電性粒子對於外部環境之耐受性提高，銅-錫層難以氧化，難以引起由銅-錫層中之銅與構成上述第2導電層之金屬(鈀等)間之賈法尼反應所導致的銅之腐蝕。因此，可進一步提高導電性粒子之導電層整體之導電性。
上述第2導電層之平均厚度較佳為500 nm以下。若上述第2導電層之平均厚度為500 nm以下，則導電性粒子之成本降低。進而，可減少構成上述第2導電層之金屬之使用量，因此可降低環境負荷。
上述鈀層之平均厚度之較佳之下限為10 nm，更佳之上限為400 nm。若鈀層之平均厚度為10 nm以上，則可進一步提高導電性粒子之導電性。
如導電性粒子11般，本發明之導電性粒子較佳為於表面具有突起。上述銅-錫層之維氏硬度(Hv)較佳為100以上，且較佳為上述導電性粒子於表面具有突起。導電性粒子較佳為於導電層之表面具有突起，進而較佳為於銅-錫層或上述第2導電層(鈀層等)之表面具有突起。上述突起較佳為複數個。大多情況下於由導電性粒子連接之電極之表面形成有氧化覆膜。於使用具有突起之導電性粒子之情形時，藉由於電極間配置並壓接導電性粒子而利用突起有效地去除上述氧化覆膜。因此，可更確實地使電極與導電性粒子之導電層接觸，可降低電極間之連接電阻。進而，於導電性粒子於表面具備絕緣性物質(絕緣性樹脂層或絕緣性粒子等)之情形時，或於導電性粒子分散於樹脂中而用作異向性導電材料之情形時，藉由導電性粒子之突起，可有效地去除導電性粒子與電極間之樹脂。因此，可提高電極間之導通可靠性。
作為於上述導電性粒子之表面形成突起之方法，可列舉：使芯物質附著於基材粒子之表面後，藉由非電解鍍敷而形成導電層之方法；以及藉由非電解鍍敷而於基材粒子之表面形成導電層後，使芯物質附著，進而藉由非電解鍍敷而形成導電層之方法等。
作為使芯物質附著於上述基材粒子之表面之方法，例如可列舉：於基材粒子之分散液中添加成為芯物質之導電性物質，藉由例如凡得瓦耳力而使芯物質集聚、附著於基材粒子的表面之方法；以及於裝有基材粒子之容器中添加成為芯物質之導電性物質，藉由容器之旋轉等之機械性作用而使芯物質附著於基材粒子的表面之方法等。其中，為了易控制附著之芯物質之量，較佳為使芯物質集聚、附著於分散液中之基材粒子的表面之方法。
作為構成上述芯物質之導電性物質，例如可列舉金屬、金屬之氧化物、石墨等導電性非金屬及導電性聚合物等。作為導電性聚合物，可列舉聚乙炔等。其中，由於可提高導電性，故而較佳為金屬。
作為上述金屬，例如可列舉：金、銀、銅、鉑、鋅、鐵、鉛、錫、鋁、鈷、銦、鎳、鉻、鈦、銻、鉍、鍺及鎘等金屬，以及錫-鉛合金、錫-銅合金、錫-銀合金及錫-鉛-銀合金等由2種類以上之金屬所構成之合金等。其中，較佳為鎳、銅、銀或金。構成上述芯物質之金屬可與構成上述導電層之金屬相同，亦可不同。又，作為上述金屬之氧化物，可列舉氧化鋁、二氧化矽及氧化鋯等。
如導電性粒子11般，本發明之導電性粒子較佳為具備配置於上述銅-錫層或鈀層之表面上之絕緣性物質。於此情形時，若將導電性粒子用於電極間之連接，則可防止鄰接之電極間之短路。具體而言，於接觸複數個導電性粒子時，在複數個電極間存在絕緣性物質，因此可防止於橫方向上相鄰之電極間之短路而並非上下電極間之短路。再者，於電極間之連接時，藉由以2個電極對導電性粒子加壓，可容易地去除導電性粒子之導電層與電極間之絕緣性物質。於導電性粒子於鈀層之表面具有突起之情形時，可更容易地去除導電性粒子之導電層與電極間之絕緣性物質。上述絕緣性物質較佳為絕緣性樹脂層或絕緣性粒子。該絕緣性粒子較佳為絕緣性樹脂粒子。
作為上述絕緣性物質之具體例，可列舉：聚烯烴類、(甲基)丙烯酸酯聚合物、(甲基)丙烯酸酯共聚物、嵌段聚合物、熱塑性樹脂、熱塑性樹脂之交聯物、熱硬化性樹脂及水溶性樹脂等。
作為上述聚烯烴類，可列舉聚乙烯、乙烯-乙酸乙烯酯共聚物及乙烯-丙烯酸酯共聚物等。作為上述(甲基)丙烯酸酯聚合物，可列舉聚(甲基)丙烯酸甲酯、聚(甲基)丙烯酸乙酯及聚(甲基)丙烯酸丁酯等。作為上述嵌段聚合物，可列舉聚苯乙烯、苯乙烯-丙烯酸酯共聚物、SB(Styrene-Butadien，苯乙烯-丁二烯)型苯乙烯-丁二烯嵌段共聚物、及SBS(Styrene-Butadien-Styrene，苯乙烯-丁二烯-苯乙烯)型苯乙烯-丁二烯嵌段共聚物、以及該等之氫化物等。作為上述熱塑性樹脂，可列舉乙烯聚合物及乙烯共聚物等。作為上述熱硬化性樹脂，可列舉環氧樹脂、酚系樹脂及三聚氰胺樹脂等。作為上述水溶性樹脂，可列舉聚乙烯醇、聚丙烯酸、聚丙烯醯胺、聚乙烯吡咯烷酮、聚氧化乙烯及甲基纖維素等。本發明之導電性粒子更佳為具備附著於上述導電層之表面之絕緣性粒子。於此情形時，若將導電性粒子用於電極間之連接，則不僅可更進一步防止於橫方向上鄰接之電極間之短路，而且可更進一步降低連接之上下之電極間之連接電阻。
作為使絕緣性粒子附著於上述導電層之表面之方法，可列舉化學性方法及物理性或機械性方法等。作為上述化學性方法，例如可列舉如下者：如WO 2003/25955A1中所揭示般，藉由利用凡得瓦耳力或靜電力之雜絮凝法而使絕緣性粒子附著於金屬表面粒子之導電層上，進而視需要進行化學鍵結。作為上述物理性或機械性方法，可列舉噴霧乾燥法、混成法、靜電附著法、噴霧法、浸鍍法及利用真空蒸鍍之方法等。其中，就絕緣性物質難以脫離而言，較佳為經由化學鍵結而使絕緣性物質附著於上述導電層之表面之方法。
上述絕緣性粒子之粒徑較佳為導電性粒子之粒徑之1/5以下。於此情形時，絕緣性粒子之粒徑未過大，更確實地實現導電層之電性連接。於絕緣性粒子之粒徑為導電性粒子之粒徑之1/5以下之情形時，藉由雜絮凝法而使絕緣性粒子附著時，可使絕緣性粒子有效地吸附於導電性粒子之表面上。又，上述絕緣性粒子之粒徑較佳為5 nm以上、更佳為10 nm以上，較佳為1000 nm以下、更佳為500 nm以下。若上述絕緣性粒子之粒徑為上述下限以上，則鄰接之導電性粒子間之距離與電子之跳躍距離相比增大，變得難以發生洩漏。若上述絕緣性粒子之粒徑為上述上限以下，則於熱壓接時所需之壓力及熱量減小。
上述絕緣性粒子之粒徑之CV(Coefficient of Variation，分佈係數)值較佳為20%以下。若CV值為20%以下，則導電性粒子之被覆層之厚度變均勻，於電極間進行熱壓接時易均勻地施加壓力，難以產生導通不良。再者，上述粒徑之CV值係藉由下述式而算出。
粒徑之CV值(%)=粒徑之標準偏差/平均粒徑×100
對於粒徑分佈，被覆金屬表面粒子前可利用粒度分佈計等進行測定，被覆後可利用SEM(Scanning Electronic Microscope，掃描電子顯微鏡)照片之圖像解析等進行測定。
再者，為了使導電性粒子之導電層露出，絕緣性物質之被覆率較佳為5%以上，較佳為70%以下。上述絕緣性物質之被覆率係由絕緣性物質被覆之部分占金屬表面粒子之表面積整體的面積。若上述被覆率為5%以上，則鄰接之導電性粒子彼此藉由絕緣性物質而更確實地絕緣。若上述被覆率為70%以下，則於電極之連接時無需施加必要以上之熱及壓力，抑制由去除之絕緣性物質導致之黏合樹脂之性能之下降。
作為上述絕緣性粒子，並無特別限定，可使用公知之無機粒子及有機高分子粒子。作為上述無機粒子，可列舉氧化鋁、二氧化矽及氧化鋯等絕緣性無機粒子。
上述有機高分子粒子較佳為使一種或二種以上具有不飽和雙鍵之單體(共)聚合而成之樹脂粒子。作為上述具有不飽和雙鍵之單體，可列舉：(甲基)丙烯酸，(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸縮水甘油酯、四羥甲基甲烷四(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、三(甲基)丙烯酸甘油酯、(聚)乙二醇二(甲基)丙烯酸酯、(聚)丙二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯等(甲基)丙烯酸酯類，乙烯基醚類，氯乙烯，苯乙烯、二乙烯苯等苯乙烯系化合物，丙烯腈等。其中可較佳地使用(甲基)丙烯酸酯類。
上述絕緣性粒子為了藉由雜絮凝而附著於導電性粒子之導電層，較佳為具有極性官能基。作為該極性官能基，例如可列舉銨基、鋶基、磷酸基及羥基矽烷基等。上述極性官能基可藉由使具有上述極性官能基及不飽和雙鍵之單體共聚合而導入。
作為具有上述銨基之單體，可列舉甲基丙烯酸N,N-二甲胺基乙酯、N,N-二甲胺基丙基丙烯醯胺及N,N,N-三甲基-N-2-甲基丙烯醯氧基乙基氯化銨等。作為具有上述鋶基之單體，可列舉甲基丙烯酸苯基二甲基鋶甲基硫酸鹽等。作為具有上述磷酸基之單體，可列舉酸性甲基丙烯酸磷醯氧基乙酯、酸性甲基丙烯酸磷醯氧基丙酯、酸性磷醯氧基聚氧乙烯醇單甲基丙烯酸酯及酸性磷醯氧基聚氧丙烯醇單甲基丙烯酸酯等。作為具有上述羥基矽烷基之單體，可列舉乙烯三羥基矽烷及3-甲基丙烯醯氧基丙基三羥基矽烷等。
作為將極性官能基導入上述絕緣性粒子之表面之其他方法，可列舉：使用具有極性基之自由基起始劑作為使上述具有不飽和雙鍵之單體聚合時之起始劑的方法。作為上述自由基起始劑，例如可列舉2,2'-偶氮雙{2-甲基-N-[2-(1-羥基丁基)]-丙醯胺}、2,2'-偶氮雙[2-(2-咪唑啉-2-基)丙烷]及2,2'-偶氮雙(2-脒基丙烷)及該等之鹽等。
(異向性導電材料)
本發明之異向性導電材料含有上述導電性粒子及黏合樹脂。
上述黏合樹脂並無特別限定。作為上述黏合樹脂，通常使用絕緣性樹脂。作為上述黏合樹脂，例如可列舉乙烯樹脂、熱塑性樹脂、硬化性樹脂、熱塑性嵌段共聚物及彈性體等。上述黏合樹脂可僅使用1種，亦可併用2種以上。
作為上述乙烯樹脂，例如可列舉乙酸乙烯酯樹脂、丙烯酸系樹脂及苯乙烯樹脂等。作為上述熱塑性樹脂，例如可列舉聚烯烴樹脂、乙烯-乙酸乙烯酯共聚物及聚醯胺樹脂等。作為上述硬化性樹脂，例如可列舉環氧樹脂、胺基甲酸酯樹脂、聚醯亞胺樹脂及不飽和聚酯樹脂等。再者，上述硬化性樹脂可為常溫硬化性樹脂、熱硬化性樹脂、光硬化性樹脂或濕氣硬化性樹脂。上述硬化性樹脂亦可與硬化劑併用。作為上述熱塑性嵌段共聚物，例如可列舉苯乙烯-丁二烯-苯乙烯嵌段共聚物、苯乙烯-異戊二烯-苯乙烯嵌段共聚物、苯乙烯-丁二烯-苯乙烯嵌段共聚物之氫化物及苯乙烯-異戊二烯-苯乙烯嵌段共聚物之氫化物等。作為上述彈性體，例如可列舉苯乙烯-丁二烯共聚橡膠及丙烯腈-苯乙烯嵌段共聚橡膠等。
上述異向性導電材料除含有上述導電性粒子及上述黏合樹脂以外，亦可含有例如填充劑、增量劑、軟化劑、塑化劑、聚合觸媒、硬化觸媒、著色劑、抗氧化劑、熱穩定劑、光穩定劑、紫外線吸收劑、潤滑劑、抗靜電劑及阻燃劑等各種添加劑。
使上述導電性粒子分散於上述黏合樹脂中之方法並無特別限定，可使用先前公知之分散方法。作為使上述導電性粒子分散於上述黏合樹脂中之方法，例如可列舉：於上述黏合樹脂中添加上述導電性粒子後，以行星式混合機等進行混練而使其分散的方法；使用均質機等使上述導電性粒子均勻地分散於水或有機溶劑中後，添加於上述黏合樹脂中，並以行星式混合機等進行混練而使其分散之方法；以及以水或有機溶劑等將上述黏合樹脂稀釋後，添加上述導電性粒子，並以行星式混合機等進行混練而使其分散之方法等。
本發明之異向性導電材料可用作異向性導電膏及異向性導電膜。於本發明之異向性導電材料為異向性導電膜之情形時，亦可於含有導電性粒子之異向性導電膜中積層不含導電性粒子之膜。
就抑制於連接構造體中之連接部產生空隙而進一步提高導通可靠性之觀點而言，上述異向性導電材料較佳為異向性導電膏。上述異向性導電材料較佳為，為異向性導電膏且以膏狀之狀態塗佈於連接對象構件之上表面者。
於上述異向性導電材料100重量%中，上述黏合樹脂之含量較佳為10~99.99重量%之範圍內。上述黏合樹脂之含量之更佳之下限為30重量%、進而較佳之下限為50重量%、尤佳之下限為70重量%，更佳之上限為99.9重量%。若上述黏合樹脂之含量滿足上述下限及上限，則可將導電性粒子有效地配置於電極間，可進一步提高電極間之導通可靠性。
於上述異向性導電材料100重量%中，上述導電性粒子之含量較佳為0.01~20重量%之範圍內。上述導電性粒子之含量之更佳之下限為0.1重量%，更佳之上限為10重量%。若上述導電性粒子之含量滿足上述下限及上限，則可進一步提高電極間之導通可靠性。
(連接構造體)
藉由使用本發明之導電性粒子或含有該導電性粒子及黏合樹脂之異向性導電材料將連接對象構件連接，可獲得連接構造體。
上述連接構造體較佳為，具備第1連接對象構件、第2連接對象構件、及連接該第1、第2連接對象構件之連接部，且該連接部藉由本發明之導電性粒子而形成，或藉由含有該導電性粒子及黏合樹脂之異向性導電材料而形成者。於使用導電性粒子之情形時，連接部本身為導電性粒子。即，第1、第2連接對象構件藉由導電性粒子而連接。
圖3中，模式性地以正面剖面圖表示使用本發明之一實施形態之導電性粒子的連接構造體。
圖3所示之連接構造體21具備第1連接對象構件22、第2連接對象構件23、連接第1、第2連接對象構件22、23之連接部24。連接部24係藉由使含有導電性粒子1之異向性導電材料硬化而形成。再者，圖3中，導電性粒子1為了方便圖示係以略圖表示。除了導電性粒子1，亦可使用導電性粒子11、61、71。
第1連接對象構件22於上表面22a上具有複數個電極22b。第2連接對象構件23於下表面23a上具有複數個電極23b。電極22b及電極23b藉由1個或複數個導電性粒子1而電性連接。因此，第1、第2連接對象構件22、23藉由導電性粒子1而電性連接。
上述連接構造體之製造方法並無特別限定。作為連接構造體之製造方法之一例，可列舉：於第1連接對象構件與第2連接對象構件間配置上述異向性導電材料而獲得積層體後，對該積層體加熱及加壓之方法等。
上述加壓之壓力為9.8×104~4.9×106 Pa左右。上述加熱之溫度為120~220℃左右。藉由使用本發明之導電性粒子，即便施加此種壓力，亦難以於銅-錫層中產生較大之裂痕。因此，可提高電極間之導通可靠性。
作為上述連接對象構件，具體而言可列舉：半導體晶片、電容器及二極管等電子零件，以及印刷基板、可撓性印刷基板及玻璃基板等電路基板等。
作為設置於上述連接對象構件上之電極，可列舉：金電極、鎳電極、錫電極、鋁電極、銅電極、鉬電極及鎢電極等金屬電極。於上述連接對象構件為可撓性印刷基板之情形時，上述電極較佳為金電極、鎳電極、錫電極或銅電極。於上述連接對象構件為玻璃基板之情形時，上述電極較佳為鋁電極、銅電極、鉬電極或鎢電極。再者，於上述電極為鋁電極之情形時，可為僅由鋁形成之電極，亦可為於金屬氧化物層之表面上積層有鋁層之電極。作為上述金屬氧化物，可列舉摻雜有3價金屬元素之氧化銦及摻雜有3價金屬元素之氧化鋅等。作為上述3價金屬元素，可列舉Sn、Al及Ga等。
若列舉本發明之導電性粒子之其他使用形態，則亦可使用導電性粒子作為用以進行構成液晶顯示元件之上下基板間之電性連接的導通材料。存在：使導電性粒子混合並分散於熱硬化性樹脂或熱UV(Ultraviolet，紫外線)併用硬化性樹脂中，以點狀塗佈於單側基板上而使其與對向基板貼合之方法；以及使導電性粒子混合並分散於周邊密封劑中，以線狀塗佈而兼作密封條及上下基板之電性連接之方法等。此種使用形態中之任一者均可應用本發明之導電性粒子。又，本發明之導電性粒子由於在基材粒子之表面設置導電層，故而藉由基材粒子之優異之彈性，可於不損傷透明基板等之情況下導電連接。
以下，列舉實施例及比較例而具體地說明本發明。本發明並不僅限定於以下之實施例。
(實施例1)
(1)樹脂粒子形成步驟
於含有3重量%之聚乙烯醇(日本合成化學工業公司製造之「GH-20」)之水溶液800重量份中添加二乙烯基苯70重量份、三羥甲基丙烷三甲基丙烯酸酯30重量份、及過氧化苯甲醯2重量份，攪拌而使其混合。於氮氣環境下一邊攪拌一邊加熱至80℃，進行15小時之反應而獲得樹脂粒子。
將所獲得之樹脂粒子以蒸餾水及甲醇清洗後，進行分離操作而獲得平均粒徑4.1 μm及變異係數5.0%之樹脂粒子。以下存在記作樹脂粒子A之情況。
(2)非電解鍍銅步驟
對所獲得之樹脂粒子A 10 g進行蝕刻處理後進行水洗。繼而，於樹脂粒子中添加硫酸鈀，使鈀離子吸附於樹脂粒子上。
繼而於含有二甲胺硼烷0.5重量%之水溶液中添加吸附有鈀離子之樹脂粒子而使鈀活化。於該樹脂粒子中添加蒸餾水500 mL而獲得粒子懸浮液。
又，準備含有40 g/L之硫酸銅(5水合物)、100 g/L之乙二胺四乙酸(EDTA，Ethylene Diamine Tetra-acetic Acid)、50 g/L之葡萄酸鈉、及25 g/L之甲醛且調整為pH 10.5之非電解鍍敷液。於上述粒子懸浮液中緩緩添加上述非電解鍍敷液，並於50℃下一面攪拌一面進行非電解鍍銅。以此種方式獲得於表面上設置有銅層(厚度約40 nm)之鍍銅粒子。
(3)非電解鍍錫步驟
製備含有氯化錫5 g及離子交換水1000 mL之溶液，混合所獲得之鍍銅粒子15 g而獲得水性懸浮液。於此水性懸浮液中加入硫脲30 g及酒石酸80 g而獲得電鍍液。將該電鍍液設為浴溫60℃並反應20分鐘。進而，於該電鍍液中進而加入氯化錫20 g、檸檬酸40 g及氫氧化鈉30 g，並於浴溫60℃下反應20分鐘，藉此獲得於銅層之表面上設置有錫層(厚度約72 nm)之粒子。
(4)合金化步驟
將所獲得之於銅層之表面上設置有錫層的粒子於220℃下加熱20小時。加熱後，銅與錫層合金化。以此種方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。於所獲得之導電性粒子中，對銅-錫層整體中所含之銅與錫之含量進行評價，結果為銅之含量為40重量%，錫之含量為60重量%。
(實施例2)
於非電解鍍銅步驟中將銅層之厚度設為約50 nm，且於非電解鍍錫步驟中將錫層之厚度變更為約60 nm，除此以外以與實施例1相同之方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為50重量%、錫之含量為50重量%。
(實施例3)
於非電解鍍銅步驟中將銅層之厚度設為約60 nm，且於非電解鍍錫步驟中將錫層之厚度變更為約48 nm，除此以外以與實施例1相同之方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為60重量%、錫之含量為40重量%。
(實施例4)
(1)芯物質附著步驟
對實施例1中所獲得之樹脂粒子A 10 g進行蝕刻處理後進行水洗。繼而，於樹脂粒子中添加硫酸鈀，使鈀離子吸附於樹脂粒子上。
於離子交換水300 mL中將附著有鈀之樹脂粒子攪拌3分鐘使其分散而獲得分散液。繼而，歷時3分鐘將金屬鎳粒子漿料(三井金屬公司製造「2020SUS」，平均粒徑200 nm)1 g添加於上述分散液中而獲得附著有芯物質之樹脂粒子。
(2)導電性粒子之製作
除使用附著有芯物質之樹脂粒子以外以與實施例1相同之方式進行非電解鍍銅步驟、非電解鍍錫步驟及合金化步驟，而獲得於樹脂粒子之表面上設置有銅-錫層且該銅-錫層含有銅與錫之合金的導電性粒子。所獲得之導電性粒子於銅-錫層之表面具有突起。對於所獲得之導電性粒子評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為40重量%、錫之含量為60重量%。再者，求銅與錫之含量時，作為芯物質而含有之鎳除外。
(實施例5)
將樹脂粒子A變更為1,4-丁二醇二丙烯酸酯與四羥甲基甲烷四丙烯酸酯之共聚樹脂粒子(1,4-丁二醇二丙烯酸酯：四羥甲基甲烷四丙烯酸酯=95重量%：5重量%，以下存在記為樹脂粒子B之情況)，除此以外以與實施例4相同之方式獲得導電性粒子。所獲得之導電性粒子於銅-錫層之表面上具有突起。
(實施例6)
(1)絕緣性樹脂粒子之製作
於安裝有4口可分離式遮罩、攪拌翼、三向旋塞、冷卻管及溫度探針之1000 mL之可分離式燒瓶中，將含有甲基丙烯酸甲酯100 mmol、N,N,N-三甲基-N-2-甲基丙烯醯氧基乙基氯化銨1 mmol、及2,2'-偶氮雙(2-脒基丙烷)二鹽酸鹽1 mmol之單體組合物以固形物分率成為5重量%之方式添加於離子交換水中後，以200 rpm進行攪拌，並於氮氣環境下於70℃下進行24小時之聚合。反應結束後，進行冷凍乾燥而獲得於表面上具有銨基、平均粒徑220 nm及CV值10%之絕緣性樹脂粒子。
使絕緣性樹脂粒子於超音波照射下分散於離子交換水中而獲得絕緣性樹脂粒子之10重量%之水分散液。
使實施例5中所獲得之導電性粒子10 g分散於離子交換水500 mL中，並添加絕緣性樹脂粒子之水分散液4 g，於室溫下攪拌6小時。以3 μm之篩網過濾器過濾後，進而以甲醇進行清洗並乾燥而獲得附著有絕緣性樹脂粒子之導電性粒子。
藉由掃描電子顯微鏡(SEM)進行觀察，結果於導電性粒子之表面上僅形成1層絕緣性樹脂粒子之被覆層。藉由圖像解析而算出相對於距導電性粒子之中心2.5 μm之面積的絕緣性樹脂粒子之被覆面積(即絕緣性樹脂粒子之粒徑之投影面積)，結果被覆率為30%。
(實施例7)
除將樹脂粒子A變更為樹脂粒子B以外以與實施例1相同之方式獲得導電性粒子。
(實施例8)
除將實施例5中所獲得之導電性粒子變更為實施例1中所獲得之導電性粒子以外以與實施例6相同之方式獲得附著有絕緣性樹脂粒子之導電性粒子。
(實施例9)
除將實施例5中所獲得之導電性粒子變更為實施例4中所獲得之導電性粒子以外以與實施例6相同之方式獲得附著有絕緣性樹脂粒子之導電性粒子。
(實施例10)
除將實施例5中所獲得之導電性粒子變更為實施例7中所獲得之導電性粒子以外以與實施例6相同之方式獲得附著有絕緣性樹脂粒子之導電性粒子。
(實施例11)
準備實施例1中所獲得之導電性粒子。使用該導電性粒子實施以下之(1)及(2)之步驟。
(1)非電解鍍鈀步驟
利用超音波處理機使所獲得之鍍銅粒子10 g分散於離子交換水500 mL中而獲得粒子懸浮液。
又，準備含有4 g/L之硫酸鈀(酸酐)、2.4 g/L之乙二胺、4.0 g/L之硫酸肼及3.5 g/L之次亞磷酸鈉且調整為pH 10之非電解鍍敷液。對上述粒子懸浮液於50℃下一面攪拌一面緩緩添加上述非電解鍍敷液，進行非電解鍍鈀。非電解鍍敷液之添加量係以鈀層之厚度成為10 nm之方式進行調整。以蒸餾水及甲醇將所獲得之經鍍鈀之樹脂粒子清洗後，進行真空乾燥。以此種方式獲得於樹脂粒子之表面上設置有銅層且於銅層之表面上設置有鈀層之導電性粒子。
(2)氯清洗去除步驟
使所獲得之導電性粒子1 g分散於蒸餾水1000 mL(比電阻為18 MΩ)中，裝入帶有攪拌機之高壓釜中並於0.1 MPa之加壓下、於121℃下攪拌清洗10小時。其後，進行過濾並乾燥。
以此種方式獲得，於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)，且該銅-錫層含有銅與錫之合金，進而於銅-錫層之表面上設置有鈀層(厚度為10 nm)的導電性粒子。
(實施例12)
準備實施例1中所獲得之樹脂粒子A。又，準備銅粉(粒徑為3.0~7.0 μm)及錫粉(粒徑為3.0~7.0 μm)。
利用樹脂粒子A、銅粉及錫粉，使用混合器(奈良機械製作所公司製造)並藉由物理性/機械性混成法，而獲得於樹脂粒子之表面上具有銅-錫層(厚度100 nm)之粒子。
繼而，將所獲得之於樹脂粒子之表面上具有銅-錫層之粒子於220℃下加熱20小時。加熱後，銅與錫層合金化。以此種方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為40重量%、錫之含量為60重量%。上述銅-錫層中之最大厚度為最小厚度之2倍以上。
(實施例13)
準備實施例1中所使用之樹脂粒子A。又，準備銅錫合金粉(銅之含量為40重量%、錫之含量為60重量%、粒徑為3.0~7.0 μm)。
利用樹脂粒子A及銅錫合金粉，使用混合器(奈良機械製作所公司製造)並藉由物理性/機械性混成法，而獲得於樹脂粒子之表面上具有銅-錫層(厚度100 nm)之粒子。
對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為40重量%、錫之含量為60重量%。上述銅-錫層中之最大厚度為最小厚度之2倍以上。
(比較例1)
準備實施例1中所獲得之樹脂粒子A。對該樹脂粒子A 10 g進行蝕刻處理後進行水洗。繼而，於樹脂粒子中添加硫酸鈀，使鈀離子吸附於樹脂粒子。
繼而於含有0.5重量%之二甲胺硼烷之水溶液中添加吸附有鈀離子之樹脂粒子而使鈀活化。於該樹脂粒子中添加蒸餾水500 mL而獲得粒子懸浮液。
又，準備含有40 g/L之硫酸銅(5水合物)、100 g/L之乙二胺四乙酸(EDTA)、50 g/L之葡萄酸鈉及25 g/L之甲醛且調整為pH 10.5的非電解鍍敷液。於上述粒子懸浮液中緩緩添加上述非電解鍍敷液，並於50℃下一面攪拌一面進行非電解鍍銅。以此種方式獲得於表面上設置有銅層(厚度100 nm)之鍍銅粒子(導電性粒子)。於比較例1中，於銅層之表面上未設置錫層。
(比較例2)
將實施例1之非電解鍍錫步驟後所獲得之於銅層(厚度約40 nm)之表面上設置有錫層(厚度約72 nm)之粒子設為導電性粒子。於比較例2中未進行合金化步驟。
(比較例3)
於非電解鍍銅步驟中將銅層之厚度設為約80 nm，且於非電解鍍錫步驟中將錫層之厚度變更為約20 nm，除此以外以與實施例1相同之方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為80重量%、錫之含量為20重量%。
(比較例4)
於非電解鍍銅步驟中將銅層之厚度設為約14 nm，且於非電解鍍錫步驟中將錫層之厚度變更為約96 nm，除此以外以與實施例1相同之方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為15重量%、錫之含量為85重量%。
(實施例14)
於非電解鍍銅步驟中將銅層之厚度設為約30 nm，且於非電解鍍錫步驟中將錫層之厚度變更為約84 nm，除此以外以與實施例1相同之方式獲得於樹脂粒子之表面上設置有銅-錫層(厚度約100 nm)且該銅-錫層含有銅與錫之合金的導電性粒子。對於所獲得之導電性粒子，評價銅-錫層整體中所含之銅與錫之含量，結果銅之含量為30重量%、錫之含量為70重量%。
(評價)
(1)導電層之裂痕
準備形成有L/S為100 μm/100 μm之銅電極之2片基板。又，準備含有導電性粒子10重量份、作為黏合樹脂之環氧樹脂(三井化學公司製造之「Sturct Bond XN-5A」)85重量份、及咪唑型硬化劑5重量份之異向性導電膏。
以導電性粒子接觸銅電極之方式於基板之上表面塗佈異向性導電膏後，以銅電極接觸導電性粒子之方式積層其他基板，施加3 MPa之壓力而進行壓接，而獲得積層體。其後，將積層體於180℃下加熱1分鐘，藉此使異向性導電膏硬化而獲得連接構造體。
對於所獲得之連接構造體，評價於導電性粒子之導電層中是否存在裂痕。以下述基準判定導電層之裂痕。
[導電層之裂痕之判定基準]
○：於導電層中無較大之裂痕，樹脂粒子未露出
△：於導電層中存在較大之裂痕，樹脂粒子少許露出
×：於導電層中存在較大之裂痕，樹脂粒子較大地露出
(2)導通可靠性
藉由四端子法對上述(1)之評價中所獲得之100個連接構造體的相對向之電極間之連接電阻進行測定，評價電極間是否導通，以下述基準判定導通可靠性。
[導通可靠性之判定基準]
○：100個連接構造體全部導通
△：100個連接構造體內未導通之數量為1個或2個
×：100個連接構造體內未導通之數量為3個以上
(3)維氏硬度
使用維氏硬度計(島津製作所公司製造之「DUH-W201」)測定所獲得之導電性粒子中之銅-錫層之維氏硬度。以下述基準判定維氏硬度。
[維氏硬度之判定基準]
A：維氏硬度超過500
B：維氏硬度為100以上、500以下
C：維氏硬度未達100
(4)熔點
於鋁鍋中裝入導電性粒子0.2~0.5 mg，使用TA Instruments製造之「DSC2920」於升溫速度為10℃/min之條件下進行掃描而獲得Heat-Flow曲線(Heat-Flow Curve，熱流曲線)。將該曲線上可見熔解之波峰之頂點所示之溫度值設為熔點。
(5)金屬含量之分析
於玻璃製三角燒瓶中，將導電性粒子0.5 g及王水(35%之鹽酸溶液15 mL、70%之硝酸5 mL)20 mL混合，於70℃之溫水浴中加溫且放置15分鐘。將燒瓶自水浴中取出後，以燒瓶中之液溫成為40℃以下之方式使其自然冷卻。冷卻後，使用玻璃漏斗及濾紙(Advantec製造之濾紙，No. 5C)過濾含有金屬離子及樹脂粒子之酸性溶液。進行固液分離，取出含有金屬離子之酸性溶液100 mL，其後以微量吸液管分取1 mL，並以純水稀釋100倍，而獲得稀釋液。使用所獲得之稀釋液以ICP(電感耦合電漿，堀場製作所製造之「ULTIMA2」)進行測量，根據所獲得之金屬離子濃度計算導電層之金屬之重量及各金屬之分量。
將結果示於下述表1中。於下述表1中，「-」表示未作評價。
1．．．導電性粒子
2．．．基材粒子
2a．．．表面
3．．．銅-錫層
3a．．．表面
11．．．導電性粒子
11a．．．表面
12．．．銅-錫層
12a．．．表面
13．．．芯物質
14．．．突起
15．．．絕緣性粒子
21．．．連接構造體
22．．．第1連接對象構件
22a．．．上表面
22b．．．電極
23．．．第2連接對象構件
23a．．．下表面
23b．．．電極
24．．．連接部
51．．．導電性粒子
52．．．銅層
52a．．．表面
53．．．錫層
61．．．導電性粒子
62．．．第2導電層
71．．．導電性粒子
72．．．銅-錫層
圖1係表示本發明之第1實施形態之導電性粒子的剖面圖。
圖2係表示本發明之第2實施形態之導電性粒子的剖面圖。
圖3係模式性地表示使用本發明之第1實施形態之導電性粒子之連接構造體的正面剖面圖。
圖4係用以說明獲得圖1所示之導電性粒子之方法的剖面圖。
圖5係表示本發明之第3實施形態之導電性粒子的剖面圖。
圖6係表示本發明之第4實施形態之導電性粒子的剖面圖。
1．．．導電性粒子
2．．．基材粒子
2a．．．表面
3．．．銅-錫層
3a．．．表面

Claims (8)

  1. 一種導電性粒子，其具備基材粒子、及設置於該基材粒子之表面上之含有銅與錫的銅-錫層，且上述銅-錫層含有銅與錫之合金，上述銅-錫層整體中之上述銅之含量超過20重量%且為75重量%以下，並且錫之含量為25重量%以上且未達80重量%。
  2. 如請求項1之導電性粒子，其中上述銅-錫層之熔點為550℃以上。
  3. 如請求項1或2之導電性粒子，其中上述銅-錫層整體中之銅之含量為40重量%以上、60重量%以下，且錫之含量為40重量%以上、60重量%以下。
  4. 如請求項1或2之導電性粒子，其於表面上具有突起。
  5. 如請求項1或2之導電性粒子，其具備配置於上述銅-錫層之表面上之絕緣性物質。
  6. 如請求項5之導電性粒子，其中上述絕緣性物質為絕緣性粒子。
  7. 一種異向性導電材料，其含有如請求項1至6中任一項之導電性粒子、及黏合樹脂。
  8. 一種連接構造體，其具備第1連接對象構件、第2連接對象構件、及連接該第1、第2連接對象構件之連接部，且上述連接部係藉由如請求項1至6中任一項之導電性粒子而形成，或藉由含有該導電性粒子及黏合樹脂之異向性導電材料而形成。
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