TWI604469B - Conductive particles, conductive materials, and connection structures - Google Patents

Conductive particles, conductive materials, and connection structures Download PDF

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Publication number
TWI604469B
TWI604469B TW102135716A TW102135716A TWI604469B TW I604469 B TWI604469 B TW I604469B TW 102135716 A TW102135716 A TW 102135716A TW 102135716 A TW102135716 A TW 102135716A TW I604469 B TWI604469 B TW I604469B
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Taiwan
Prior art keywords
conductive
particles
conductive layer
layer
resin
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TW102135716A
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English (en)
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TW201421491A (zh
Inventor
Keizo Nishioka
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Sekisui Chemical Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/18—Non-metallic particles coated with metal
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
    • H—ELECTRICITY
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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Description

導電性粒子、導電材料及連接構造體
本發明係關於一種於基材粒子之表面上配置有導電材之導電性粒子。更為詳細而言，本發明例如關於一種可用於電極間之電性連接之導電性粒子。又，本發明係關於一種使用上述導電性粒子之導電材料及連接構造體。
各向異性導電膏及各向異性導電膜等導電材料已廣為人知。該等各向異性導電材料中，於黏合劑樹脂中分散有導電性粒子。
為了獲得各種連接構造體，上述各向異性導電材料例如被用於軟性印刷基板與玻璃基板之連接(FOG(Film on Glass，鍍膜玻璃))、半導體晶片與軟性印刷基板之連接(COF(Chip on Film，薄膜覆晶))、半導體晶片與玻璃基板之連接(COG(Chip on Glass，玻璃覆晶))、以及軟性印刷基板與環氧玻璃基板之連接(FOB(Film on Board，鍍膜板))等。
作為上述導電性粒子之一例，下述專利文獻1中揭示有具備複合粒子與覆蓋該複合粒子之金屬鍍層的導電性粒子。上述複合粒子具有塑膠核體、與藉由化學鍵結而吸附於該塑膠核體之非導電性無機粒子。
下述專利文獻2中揭示有如下導電性粒子，其具備塑膠核體、覆蓋該塑膠核體之高分子電解質層、經由該高分子電解質層而吸附於上述塑膠核體之金屬粒子、及以覆蓋該金屬粒子之方式形成於上述塑膠 核體周圍之無電鍍金屬層。專利文獻2中記載，吸附於上述塑膠核體之金屬粒子為例如選自金、銀、銅、鈀及鎳中之金屬之粒子。
下述專利文獻3中揭示有如下導電性粒子，其係於基材粒子之表面形成有含有鎳及磷之金屬鍍敷被膜層與金層之多層導電層。該導電性粒子中，於基材粒子之表面上配置有芯物質，且該芯物質被導電層被覆。導電層因芯物質而隆起，於導電層之表面形成有突起。專利文獻3中，於構成上述芯物質之導電性物質為金屬之情形時，作為該金屬，例如可列舉：鎳、銅、金、銀、鉑、鋅、鐵、鉛、錫、鋁、鈷、銦、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種以上金屬構成之合金等。
[先前技術文獻] [專利文獻]
[專利文獻1]日本專利特開2011-29179號公報
[專利文獻2]日本專利特開2011-108446號公報
[專利文獻3]日本專利特開2006-228475號公報
上述專利文獻1~3中揭示有於導電層之外側之表面具有突起之導電性粒子。多數情況下，於由導電性粒子連接之電極、及導電性粒子之導電層之表面形成有氧化被膜。上述導電層之突起係為了於經由導電性粒子將電極間壓接時將電極及導電性粒子之表面之氧化被膜去除而使導電層與電極接觸而形成。
然而，於使用如專利文獻1~3所記載之先前之導電性粒子而將電極間連接的情形時，有連接電阻變高之情況。又，無法將電極及導電性粒子之表面之氧化被膜充分地去除，而連接電阻容易變得相對較高。
又，近年來，期待一種可使電極間之連接電阻進一步變低之導電性粒子。
本發明之目的在於提供一種於將電極間連接之情形時可使電極間之連接電阻變低之導電性粒子、以及使用該導電性粒子之導電材料及連接構造體。
根據本發明之較廣態樣，提供一種導電性粒子，其具備：基材粒子、與配置於上述基材粒子之表面上之一部分區域之導電材，且上述導電材之材質為莫氏硬度高於鎳之材質。
於本發明之導電性粒子之一特定態樣中，上述導電性粒子具備：上述基材粒子、與配置於上述基材粒子之表面上之一部分區域之上述導電材，且上述導電材之材質為鉬、碳化鎢、鎢、碳化鈦或碳化鉭。
於本發明之導電性粒子之一特定態樣中，該導電性粒子具備複數之上述導電材。
於本發明之導電性粒子之一特定態樣中，該導電性粒子具備：上述基材粒子、配置於上述基材粒子之表面上之導電層、及配置於上述基材粒子之表面上之一部分區域之上述導電材，且上述導電材被埋入上述導電層內。
於本發明之導電性粒子之一特定態樣中，上述導電層於外側之表面具有突起，且於上述導電層之上述突起之內側配置有上述導電材。
於本發明之導電性粒子之一特定態樣中，上述導電層具有鎳層。
於本發明之導電性粒子之一特定態樣中，上述導電層於上述基材粒子側具有鎳層，於與上述基材粒子側相反側具有鈀層。
於本發明之導電性粒子之一特定態樣中，該導電性粒子進而具備附著於上述導電層之表面之絕緣性物質。
於本發明之導電性粒子之一特定態樣中，上述導電材為粒子。
於本發明之導電性粒子之一特定態樣中，上述導電性粒子具備：上述基材粒子、與配置於上述基材粒子之表面上之一部分區域之上述導電材，且上述導電材之材質為鉬、碳化鎢、鎢或碳化鉭。
根據本發明之較廣態樣，提供一種導電材料，其含有上述導電性粒子與黏合劑樹脂。
根據本發明之較廣態樣，提供一種連接構造體，其具備：於表面具有第1電極之第1連接對象構件、於表面具有第2電極之第2連接對象構件、及將上述第1連接對象構件與上述第2連接對象構件連接之連接部，且上述連接部由上述導電性粒子形成，或者由含有上述導電性粒子與黏合劑樹脂之導電材料形成，上述第1電極與上述第2電極藉由上述導電性粒子而電性連接。
本發明之導電性粒子係於基材粒子之表面上之一部分區域配置有導電材，且上述導電材之材質為莫氏硬度高於鎳之材質，因此於使用本發明之導電性粒子將電極間連接之情形時，可使連接電阻變低。
1‧‧‧導電性粒子
1a‧‧‧突起
2‧‧‧基材粒子
3‧‧‧導電層
3a‧‧‧突起
4‧‧‧導電材
5‧‧‧絕緣性物質
11‧‧‧導電性粒子
11a‧‧‧突起
12‧‧‧第1導電層
13‧‧‧第2導電層
13a‧‧‧突起
21‧‧‧導電性粒子
22‧‧‧導電層
51‧‧‧連接構造體
52‧‧‧第1連接對象構件
52a‧‧‧第1電極
53‧‧‧第2連接對象構件
53a‧‧‧第2電極
54‧‧‧連接部
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係表示本發明之第3實施形態之導電性粒子的剖面圖。
圖4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前視剖面圖。
以下，對本發明之詳細內容進行說明。
(導電性粒子)
本發明之導電性粒子具備：基材粒子、與配置於該基材粒子之表面上之一部分區域之導電材。上述導電材之材質為莫氏硬度高於鎳之材質。
藉由採用本發明之導電性粒子之上述構成，於使用本發明之導電性粒子將電極間連接之情形時，難以產生電極間之連接不良，進而可有效地降低電極間之連接電阻。
上述導電材之材質較佳為鉬、鎢、碳化鎢、碳化鈦或碳化鉭，亦較佳為鉬、鎢、碳化鎢、或碳化鉭。該等材質之莫氏硬度較高。於使用具備該等材質之導電材之導電性粒子將電極間連接之情形時，難以產生電極間之連接不良，進而可有效地降低電極間之連接電阻。
本發明之導電性粒子較佳為具備：上述基材粒子、配置於上述基材粒子之表面上之導電層、及配置於上述基材粒子之表面上之一部分區域之上述導電材。該情形時，上述導電材較佳為被埋入上述導電層內。上述導電層之一部分區域較佳為與上述基材粒子接觸。
藉由使用於上述導電層內埋入有上述導電材之導電性粒子，於使用導電性粒子將電極間連接之情形時，進一步難以產生電極間之連接不良，進而可進一步降低電極間之連接電阻。
本發明之導電性粒子中，較佳為上述導電層於外側之表面具有突起，且於上述導電層之上述突起之內側配置有上述導電材。較佳為由上述導電材形成上述突起。
多數情況下，於由導電性粒子連接之電極之表面形成有氧化被膜。進而，多數情況下，於上述導電層之外側之表面形成有氧化被膜。由於上述導電層於外側之表面具有複數個突起，故而於電極間配置導電性粒子後進行壓接，藉此利用突起去除氧化被膜。因此，可使電極與導電性粒子進一步確實地接觸，而可進一步降低電極間之連接 電阻。
以下，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，藉此明確本發明。
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、導電層3、複數之導電材4、及複數之絕緣性物質5。導電層3係配置於基材粒子2之表面上。導電性粒子1中，形成有單層之導電層3。導電層3被覆基材粒子2。導電層3亦被覆導電材4。導電層3於外側之表面具有複數個突起3a。
導電性粒子1具備複數之導電材4。複數之導電材4被配置於基材粒子2之表面上之一部分區域，且埋入導電層3內。導電材4並未被配置於基材粒子2之表面上之全部區域。導電材4並未被覆基材粒子2之整個表面。導電材4被配置於基材粒子2之表面上之一部分區域，故基材粒子2具有未接觸導電材4之表面區域。導電材4係配置於突起3a之內側。於1個突起3a之內側配置有1個導電材4。導電層3之外側之表面因複數之導電材4而隆起，形成複數個突起3a。導電性粒子具備複數之導電材，藉此容易於導電性粒子之外側之表面形成複數個突起。
導電材4為粒子。因導電材4為粒子，故於基材粒子2之表面上之一部分區域配置有導電材4。
導電材4接觸基材粒子2。亦可於基材粒子之表面與導電材之表面之間配置導電層。亦可導電材不接觸基材粒子，而基材粒子之表面與導電材之表面隔著距離。
絕緣性物質5係配置於導電層3之表面上。絕緣性物質5為絕緣性粒子。絕緣性物質5係由具有絕緣性之材料形成。導電性粒子亦可未必具備絕緣性物質。又，導電性粒子除具備絕緣粒子作為絕緣性物質外，亦可具備被覆導電層之外側之表面之絕緣層作為絕緣性物質。
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、第1導電層12、第2導電層13、複數之導電材4、及複數之絕緣性物質5。
導電性粒子1與導電性粒子11僅導電層不同。即，導電性粒子1形成有單層構造之導電層，相對於此，導電性粒子11形成有2層構造之第1導電層12及第2導電層13。導電材4係埋入第1導電層11及導電層13內。
第1導電層12係配置於基材粒子2之表面上。於基材粒子2與第2導電層13之間配置有第1導電層12。第1導電層12為位於基材粒子2側、且接觸基材粒子2之導電層。第2導電層13位於與基材粒子2側相反側，且未接觸基材粒子2。因此，於基材粒子2之表面上配置有第1導電層12，於第1導電層12之表面上配置有第2導電層13。第2導電層13於外表面具有複數個突起13a。導電性粒子11於導電性之表面具有複數個突起11a。
圖3係表示本發明之第3實施形態之導電性粒子的剖面圖。
圖3所示之導電性粒子21具備：基材粒子2、導電層22、及複數之導電材4。導電層22係配置於基材粒子2之表面上。導電材4係埋入導電層22內。
導電性粒子21於表面不具有突起。導電性粒子21為球狀。導電層22於外側之表面不具有突起。如此，本發明之導電性粒子亦可不具有突起而亦可為球狀。又，導電性粒子21不具有絕緣性物質。但，導電性粒子21亦可具備配置於導電層22之表面上之絕緣性物質。
以下，對導電性粒子更詳細地進行說明。
[基材粒子]
作為上述基材粒子，可列舉：樹脂粒子、除金屬粒子外之無機粒子、有機無機混合粒子及金屬粒子等。其中，較佳為除金屬粒子外 之基材粒子，更佳為樹脂粒子、除金屬粒子外之無機粒子或有機無機混合粒子。
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。作為用以形成上述樹脂粒子之樹脂，例如可列舉：聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚偏二氯乙烯、聚異丁烯、聚丁二烯等聚烯烴樹脂；聚甲基丙烯酸甲酯及聚丙烯酸甲酯等丙烯酸系樹脂；聚對苯二甲酸烷二酯、聚碳酸酯、聚醯胺、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、酚樹脂、三聚氰胺樹脂、苯并胍胺樹脂、脲樹脂、環氧樹脂、不飽和聚酯樹脂、飽和聚酯樹脂、聚對苯二甲酸乙二酯、聚碸、聚苯醚、聚縮醛、聚醯亞胺、聚醯胺醯亞胺、聚醚醚酮、聚醚碸、二乙烯苯聚合物、以及二乙烯苯系共聚物等。作為上述二乙烯苯系共聚物等，可列舉：二乙烯苯-苯乙烯共聚物及二乙烯苯-(甲基)丙烯酸酯共聚物等。因可容易地將上述樹脂粒子之硬度控制在較佳範圍內，故用以形成上述樹脂粒子之樹脂較佳為使1種或2種以上具有乙烯性不飽和基之聚合性單體聚合而成之聚合物。
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，可列舉非交聯性之單體與交聯性之單體。
作為上述非交聯性之單體，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)丙烯酸鯨蠟酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸異酯等(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、氯苯乙烯等含鹵素單體等。
作為上述交聯性之單體，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、甘油三(甲基)丙烯酸酯、甘油二(甲基)丙烯酸酯、(聚)乙二醇二(甲基)丙烯酸酯、(聚)丙二醇二(甲基)丙烯酸酯、(聚)1,4-丁二醇二(甲基)丙烯酸酯、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、偏苯三酸三烯丙酯、二乙烯苯、鄰苯二甲酸二烯丙酯、二烯丙基丙烯醯胺、二烯丙醚、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單體等。
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，藉此可獲得上述樹脂粒子。作為該方法，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、以及使用非交聯之種粒子與自由基聚合起始劑一起使單體膨潤而聚合之方法等。
於上述基材粒子為除金屬外之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形成之粒子，並無特別限定，例如可列舉：使水解性之具有2個以上烷氧基矽烷基之矽化合物水解而形成交聯聚合物粒子後，根據需要進行焙燒，藉此獲得之粒子。作為上述有機無機混合粒子，例如可列舉：由交聯而成之烷氧基矽烷基聚合物與丙烯酸系樹脂形成之有機無機混合粒子等。
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。於上述基材粒子為金屬粒子之情形時，該金屬粒子較佳為銅粒子。但，上述基材粒子較佳為並非金屬粒子。
上述基材粒子之粒徑較佳為0.1μm以上，更佳為1μm以上，進而較佳為1.5μm以上，特佳為2μm以上，且較佳為1000μm以下，更佳為500μm以下，進而較佳為300μm以下，進而更佳為50μm以下，特佳為30μm以下，最佳為5μm以下。若基材粒子之粒徑為上述下限以上，則導電性粒子與電極之接觸面積變大，因此電極間之導通可靠性進一步變高，經由導電性粒子而連接之電極間之連接電阻進一步變低。進而，於藉由無電電鍍於基材粒子之表面形成導電層時難以凝集，而難以形成凝集之導電性粒子。若粒徑為上述上限以下，則導電性粒子容易被充分地壓縮，而電極間之連接電阻進一步變低，進而電極間之間隔變小。上述基材粒子之粒徑於基材粒子為圓球狀之情形時表示直徑，於基材粒子並非圓球狀之情形時表示最大徑。
上述基材粒子之粒徑特佳為2μm以上且5μm以下。若上述基材粒子之粒徑為2~5μm之範圍內，則電極間之間隔變小，且即便使導電層之厚度變厚，亦可獲得較小之導電性粒子。上述基材粒子之粒徑亦較佳為3μm以下。
[導電層]
本發明之導電性粒子具有配置於基材粒子之表面上之導電層。
用以形成上述導電層之金屬並無特別限定。作為該金屬，例如可列舉：金、銀、鈀、銅、鉑、鋅、鐵、錫、鉛、鋁、鈷、銦、鎳、鉻、鈦、銻、鉍、鉈、鍺、鎘、矽及該等之合金等。又，作為上述金屬，可列舉摻錫氧化銦(ITO)及焊錫等。其中，因可使電極間之連接電阻進一步變低，故較佳為含有錫之合金、鎳、鈀、銅或金，更佳為 鎳或鈀。
如導電性粒子1、21般，上述導電層亦可由1層形成。如導電性粒子11般，導電層亦可由複數層形成。即，導電層亦可具有2層以上之積層構造。於導電層由複數層形成之情形時，最外層(第2導電層等)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。最外層較佳為鈀層，亦較佳為金層。於最外層為該等較佳之導電層之情形時，電極間之連接電阻進一步變低。又，於最外層為金層之情形時，耐腐蝕性進一步變高。鎳層含有50重量%以上之鎳。鈀層或金層含有50重量%以上之鈀或金。
接觸上述基材粒子之導電層較佳為含有鎳。於如導電性粒子1、21般上述導電層為單層之情形時，上述導電層較佳為含有鎳。於如導電性粒子11般導電層具有基材粒子側之第1導電層及與基材粒子側相反側之第2導電層的情形時，上述第1導電層(接觸基材粒子之導電層)較佳為含有鎳。上述導電層及上述第1導電層較佳為含有鎳作為主成分。含有鎳之導電層之導電性相對較高。因此，於藉由具備含有鎳之導電層之導電性粒子將電極間連接之情形時，電極間之連接電阻進一步變低。
接觸上述基材粒子之導電層100重量%中，鎳之含量較佳為50重量%以上。於上述導電層為單層之情形時，上述導電層100重量%中，鎳之含量較佳為50重量%以上。於上述導電層具備上述第1、第2導電層之情形時，上述第1導電層100重量%中鎳之含量較佳為50重量%以上。若鎳之含量為50重量%以上，則電極間之連接電阻充分變低。上述導電層或上述第1導電層100重量%中，鎳之含量更佳為60重量%以上，進而較佳為70重量%以上，特佳為90重量%以上。上述導電層或上述第1導電層100重量%中鎳之含量可為97重量%以上，可為97.5重量%以上，亦可為98重量%以上。上述導電層或上述第1導電層100重 量%中鎳之含量較佳為99.85重量%以下，更佳為99.7重量%以下，進而較佳為未達99.45重量%。若上述鎳之含量為上述下限以上，則電極間之連接電阻進一步變低。又，於電極或導電層之表面之氧化被膜較少之情形時，有上述鎳之含量越多電極間之連接電阻變得越低之傾向。
上述導電層或上述第1導電層較佳為含有鎳、與硼及磷中之至少1種。於上述導電層或上述第1導電層中，鎳與硼及磷中之至少1種亦可合金化。又，於上述導電層或上述第1導電層中，亦可使用鎳、硼及磷以外之成分。
又，將連接構造體置於酸之存在下時，有電極間之連接電阻上升之情況。因此，上述導電層或上述第1導電層存在較佳為於基材粒子側鎳層中之磷之含量較高、且於與基材粒子相反側鎳層中之磷之含量較低的情形。
上述導電層或上述第1導電層100重量%中，硼與磷之合計含量較佳為0.01重量%以上，更佳為0.05重量%以上，進而較佳為0.1重量%以上，且較佳為5重量%以下，更佳為4重量%以下，進而較佳為3重量%以下，特佳為2.5重量%以下，最佳為2重量%以下。若硼與磷之合計含量為上述下限以上，則上述導電層或上述第1導電層進一步變硬，可更有效地將電極及導電性粒子之表面之氧化被膜去除，而可使電極間之連接電阻進一步變低。若硼與磷之合計含量為上述上限以下，則鎳之含量相對變多，因此電極間之連接電阻變低。
上述導電層或上述第1導電層100重量%中，硼之含量較佳為0.01重量%以上，更佳為0.05重量%以上，進而較佳為0.1重量%以上，且較佳為5重量%以下，更佳為4重量%以下，進而較佳為3重量%以下，特佳為2.5重量%以下，最佳為2重量%以下。若硼之含量為上述下限以上，則上述導電層或上述第1導電層進一步變硬，可更有效地將電 極及導電性粒子之表面之氧化被膜去除，而可使電極間之連接電阻進一步變低。若硼之含量為上述上限以下，則鎳之含量相對變多，因此電極間之連接電阻變低。
上述導電層或上述第1導電層較佳為不含磷，或含有磷且上述導電層或上述第1導電層100重量%中磷之含量未達10.0重量%。上述導電層100重量%中，磷之含量更佳為未達0.5重量%，進而較佳為0.3重量%以下，特佳為0.1重量%以下。上述導電層或上述第1導電層特佳為不含磷。
上述導電層或上述第1導電層中之鎳、硼及磷等之各含量之測定方法可使用已知之各種分析法，並無特別限定。作為該測定方法，可列舉吸光分析法或光譜分析法等。於上述吸光分析法中，可使用火焰吸光光度計及電加熱爐吸光光度計等。作為上述光譜分析法，可列舉電漿發光分析法及電漿離子源質量分析法等。
對上述導電層或上述第1導電層中之鎳、硼及磷等之各含量進行測定時，較佳為使用ICP(inductively coupled plasma，電感耦合電漿)發光分析裝置。作為ICP發光分析裝置之市售品，可列舉HORIBA公司製造之ICP發光分析裝置等。
就使電極間之連接電阻進一步變低之觀點而言，上述導電層較佳為於上述基材粒子側具有鎳層，於與上述基材粒子側相反側具有第2導電層。該情形時，第2導電層較佳為鈀層或金層，更佳為鈀層，進而較佳為金層。
於上述基材粒子之表面上形成上述導電層或上述第1導電層的方法、以及於上述第1導電層之表面上形成上述第2導電層的方法並無特別限定。作為形成導電層之方法，例如可列舉：利用無電電鍍之方法、利用電鍍之方法、利用物理蒸鍍之方法、以及將金屬粉末或含有金屬粉末與黏合劑之漿料塗佈於基材粒子或其他導電層之表面的方法 等。其中，因導電層之形成較為簡單，故較佳為利用無電電鍍之方法。作為上述利用物理蒸鍍之方法，可列舉真空蒸鍍、離子鍍著及離子濺鍍等方法。
上述導電性粒子之粒徑較佳為0.5μm以上，更佳為1μm以上，且較佳為100μm以下，更佳為20μm以下。若導電性粒子之粒徑為上述下限以上及上限以下，則於使用導電性粒子將電極間連接之情形時，導電性粒子與電極之接觸面積充分變大，且於形成導電層時難以形成凝集之導電性粒子。又，經由導電性粒子而連接之電極間之間隔未變得過大，且導電層變得難以自基材粒子之表面剝離。
上述導電性粒子之粒徑於導電性粒子為圓球狀之情形時表示直徑，於導電性粒子並非圓球狀之情形時表示最大徑。
導電性粒子中之導電層整體之厚度、及導電層為單層之情形之導電層之厚度較佳為0.005μm以上，更佳為0.01μm以上，進而較佳為0.05μm以上，且較佳為1μm以下，更佳為0.3μm以下。若上述導電層之厚度為上述下限以上及上述上限以下，則可獲得充分之導電性，且導電性粒子未變得過硬，而於將電極間連接時導電性粒子充分變形。
於導電層為2層以上之積層構造之情形時，接觸基材粒子之導電層(第1導電層)之厚度較佳為0.001μm以上，更佳為0.01μm以上，進而較佳為0.05μm以上，且較佳為0.5μm以下，更佳為0.3μm以下，進而較佳為0.1μm以下。若接觸基材粒子之導電層之厚度為上述下限以上及上述上限以下，則可使導電層之被覆均勻，且電極間之連接電阻充分變低。
導電性粒子中之導電層整體之厚度、及導電層為單層之情形之導電層之厚度特佳為0.05μm以上且0.3μm以下。進而，特佳為，基材粒子之粒徑為2μm以上且5μm以下，且導電性粒子中之導電層整體 之厚度、及導電層為單層之情形之導電層之厚度為0.05μm以上且0.3μm以下。該情形時，可將導電性粒子更佳地用於通過較大電流之用途。進而，於壓縮導電性粒子而將電極間連接之情形時，可進一步抑制電極損傷。
上述導電層之厚度例如可藉由使用穿透式電子顯微鏡(TEM)對導電性粒子之剖面進行觀察而測定。
作為控制上述導電層及上述第1導電層中之鎳、硼及磷之含量的方法，例如可列舉：於藉由無電鍍鎳形成導電層時控制鎳鍍液之pH值的方法；於藉由無電鍍鎳形成導電層時調整含硼還原劑之濃度的方法；於藉由無電鍍鎳形成導電層時調整含磷還原劑之濃度的方法；以及調整鎳鍍液中之鎳濃度之方法等。
於藉由無電電鍍形成之方法中，通常進行觸媒化步驟與無電電鍍步驟。以下，對藉由無電電鍍而於樹脂粒子之表面形成含有鎳與硼之合金鍍層之方法的一例進行說明。
上述觸媒化步驟中，使成為用以藉由無電電鍍形成鍍層之起點的觸媒形成於樹脂粒子之表面。
作為使上述觸媒形成於樹脂粒子表面之方法，例如可列舉：於含有氯化鈀與氯化錫之溶液中添加樹脂粒子後，利用酸溶液或鹼溶液使樹脂粒子之表面活化，而使鈀析出至樹脂粒子之表面的方法；以及於含有硫酸鈀與胺基吡啶之溶液中添加樹脂粒子後，利用含有還原劑之溶液使樹脂粒子之表面活化，而使鈀析出至樹脂粒子之表面的方法等。可較佳地使用含硼還原劑作為上述還原劑。又，藉由使用含磷還原劑作為上述還原劑，可形成含磷之導電層。
於上述無電電鍍步驟中，可較佳地使用含有含鎳化合物及上述含硼還原劑之鎳鍍浴。藉由將樹脂粒子浸漬於鎳鍍浴中，而可使鎳析出至表面上形成有觸媒之樹脂粒子之表面，可形成含有鎳與硼之導電 層。
作為上述含鎳化合物，可列舉硫酸鎳及氯化鎳等。上述含鎳化合物較佳為鎳鹽。
作為上述含硼還原劑，可列舉二甲胺硼烷、硼氫化鈉及硼氫化鉀等。作為上述含磷還原劑，可列舉次亞磷酸鈉等。
[導電材]
本發明之導電性粒子具備配置於基材粒子之表面上之導電材。該導電材之材質較佳為鉬(Mo)(莫氏硬度5.5)、鎢(W)(莫氏硬度7.5)、碳化鎢(WC)(莫氏硬度9)、碳化鈦(TiC)(莫氏硬度9)、或碳化鉭(TaC)(莫氏硬度9)。導電性粒子具備上述特定材質之導電材，藉此導電性粒子之導電性之表面充分變硬，而可使電極間之連接電阻充分變低。上述導電材之材質之莫氏硬度高於鎳(Ni)(莫氏硬度5.0)之莫氏硬度。上述導電材之材質較佳為碳化鎢或碳化鉭。上述導電材之材質較佳為鉬，更佳為鎢，更佳為碳化鎢，更佳為碳化鈦，進而較佳為碳化鉭。
上述導電材之粉體電阻率之值較佳為0.1Ω‧cm以下。
本發明之導電性粒子較佳為於導電性之表面具有突起。上述導電層較佳為於外側之表面具有突起。該突起較佳為複數個。多數情況下，於由導電性粒子連接之電極之表面形成有氧化被膜。進而，多數情況下，於導電性粒子之導電層之表面形成有氧化被膜。藉由使用具有突起之導電性粒子，而於電極間配置導電性粒子後進行壓接，藉此利用突起有效地將氧化被膜去除。於上述突起之內側存在特定材質之上述導電材，藉此變得容易利用突起將氧化被膜充分地去除。因此，可使電極與導電性粒子進一步確實地接觸，而可使電極間之連接電阻變低。進而，於導電性粒子於表面具有絕緣性物質之情形時，或導電性粒子被分散於黏合劑樹脂中而用作導電材料之情形時，利用導電性 粒子之突起，可有效地去除導電性粒子與電極之間之樹脂。因此，可提高電極間之導通可靠性。
藉由將上述導電材埋入上述導電層中，容易使上述導電層於外側之表面具有複數個突起。
於上述導電性粒子具備上述導電層之情形時，上述導電材可接觸上述基材粒子，亦可不接觸上述基材粒子。亦可於上述基材粒子與上述導電材之間配置有上述導電層之一部分。
本發明之導電性粒子較佳為具備複數之上述導電材。該情形時，由於在導電層之內側配置有複數之上述導電材的部位，而可使導電性粒子之導電部變硬。又，容易於導電性粒子及導電層之表面形成複數個突起。
上述導電材較佳為粒子。該情形時，因配置於導電層之內側之作為粒子之導電材的形狀，可有效地使導電性粒子之導電部變硬。又，容易於導電性粒子及導電層之表面形成複數個突起。
作為粒子之上述導電材之形狀較佳為塊狀。關於作為粒子之上述導電材，例如可列舉：粒子狀之塊、複數個微小粒子凝集而成之凝集塊、及不定形之塊等。
將上述基材粒子之粒徑設為D時，上述導電材之最大徑較佳為0.005D以上，更佳為0.015D以上，且較佳為0.25D以下，更佳為0.15D以下。
又，將上述基材粒子之粒徑設為D時，上述導電層之厚度方向上之上述導電材之尺寸較佳為0.005D以上，更佳為0.015D以上，且較佳為0.25D以下，更佳為0.15D以下。
作為形成上述突起之方法，可列舉：使上述導電材附著於基材粒子之表面後利用無電電鍍形成導電層之方法，以及利用無電電鍍於基材粒子之表面形成導電層後使上述導電材附著，進而利用無電電鍍 形成導電層的方法等。作為形成上述突起之其他方法，可列舉：於基材粒子之表面上形成第1導電層後，於該第1導電層上配置上述導電材並繼而形成第2導電層的方法；以及於在基材粒子之表面上形成導電層之中途階段添加上述導電材的方法等。
平均1個上述導電性粒子之上述導電材之數及上述突起之數分別較佳為3個以上，更佳為5個以上。上述導電材之數及上述突起之數之上限並無特別限定。上述導電材之數及上述突起之數之上限可考慮導電性粒子之粒徑等而適當選擇。
[絕緣性物質]
本發明之導電性粒子較佳為具備配置於上述導電層之表面上之絕緣性物質。該情形時，若將導電性粒子用於電極間之連接，則可進一步防止鄰接之電極間之短路。具體而言，於複數個導電性粒子接觸時，因於複數個電極間存在絕緣性物質，故可防止並非上下之電極間而是橫方向上相鄰之電極間的短路。再者，於將電極間連接時，利用2個電極對導電性粒子進行加壓，藉此可容易地將導電性粒子之導電層與電極之間之絕緣性物質去除。於導電性粒子於導電層之外側之表面具有複數個突起之情形時，可容易地將導電性粒子之導電層與電極之間之絕緣性物質去除。
由於將電極間壓接時可更容易地將上述絕緣性物質去除，故上述絕緣性物質較佳為絕緣性粒子。
作為上述絕緣性物質之材料即絕緣性樹脂之具體例，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。
(導電材料)
本發明之導電材料含有上述之導電性粒子與黏合劑樹脂。本發 明之導電性粒子較佳為分散於黏合劑樹脂中而用作導電材料。上述導電材料較佳為各向異性導電材料。
上述黏合劑樹脂並無特別限定。可使用公知之絕緣性之樹脂作為上述黏合劑樹脂。
作為上述黏合劑樹脂，例如可列舉：乙烯基樹脂、熱塑性樹脂、硬化性樹脂、熱塑性嵌段共聚物及彈性體等。上述黏合劑樹脂可僅使用1種，亦可併用2種以上。
作為上述乙烯基樹脂，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，上述硬化性樹脂亦可為常溫硬化型樹脂、熱硬化型樹脂、光硬化型樹脂或濕氣硬化型樹脂。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-丁二烯共聚合橡膠、及丙烯腈-苯乙烯嵌段共聚合橡膠等。
上述導電材料除含有上述導電性粒子及上述黏合劑樹脂外，例如亦可含有填充劑、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劑樹脂中之方法可使用先前公知之分散方法，並無特別限定。作為使上述導電性粒子分散於上述黏合劑樹脂中之方法，例如可列舉：於上述黏合劑樹脂中添加上述導電性粒子後，利用行星式混合機等進行混練而使之分散的方法；使用 均質器等使上述導電性粒子均勻地分散於水或有機溶劑中後，添加於上述黏合劑樹脂中，利用行星式混合機等進行混練而使之分散的方法；以及利用水或有機溶劑等稀釋上述黏合劑樹脂後，添加上述導電性粒子，利用行星式混合機等進行混練而使之分散的方法等。
本發明之導電材料可用作導電膏及導電膜等。於本發明之導電材料為導電膜之情形時，亦可於該含有導電性粒子之導電膜上積層不含導電性粒子之膜。上述導電膏較佳為各向異性導電膏。上述導電膜較佳為各向異性導電膜。
上述導電材料100重量%中，上述黏合劑樹脂之含量較佳為10重量%以上，更佳為30重量%以上，進而較佳為50重量%以上，特佳為70重量%以上，且較佳為99.99重量%以下，更佳為99.9重量%以下。若上述黏合劑樹脂之含量為上述下限以上及上述上限以下，則導電性粒子有效率地配置於電極間，而由導電材料連接之連接對象構件之連接可靠性進一步變高。
上述導電材料100重量%中，上述導電性粒子之含量較佳為0.01重量%以上，更佳為0.1重量%以上，且較佳為40重量%以下，更佳為20重量%以下，進而較佳為10重量%以下。若上述導電性粒子之含量為上述下限以上及上述上限以下，則電極間之導通可靠性進一步變高。
(連接構造體)
使用本發明之導電性粒子或使用含有該導電性粒子與黏合劑樹脂之導電材料將連接對象構件進行連接，藉此可獲得連接構造體。
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、及將第1連接對象構件與第2連接對象構件連接之連接部，且該連接部由本發明之導電性粒子形成，或者由含有該導電性粒子與黏合劑樹脂之導電材料形成。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連接對象構件由導電性粒子連接。
圖4係示意性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前視剖面圖。
圖4所示之連接構造體51具備第1連接對象構件52、第2連接對象構件53、及將第1、第2連接對象構件52、53連接之連接部54。連接部54係藉由使含有導電性粒子1之導電材料硬化而形成。再者，圖4中，導電性粒子1係為了圖示之方便而簡略地表示。
第1連接對象構件52於表面(上表面)具有複數個第1電極52a。第2連接對象構件53於表面(下表面)具有複數個第2電極53a。第1電極52a與第2電極53a由1個或複數個導電性粒子1電性連接。因此，第1、第2連接對象構件52、53由導電性粒子1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連接對象構件之間配置上述導電材料而獲得積層體後，對該積層體進行加熱及加壓之方法等。上述加壓之壓力為9.8×104~4.9×106Pa左右。上述加熱之溫度為120~220℃左右。
作為上述連接對象構件，具體而言，可列舉：半導體晶片、電容器及二極體等電子零件、以及印刷基板、軟性印刷基板、環氧玻璃基板及玻璃基板等電路基板等電子零件等。上述導電材料較佳為用以連接電子零件之導電材料。上述導電材料較佳為漿料狀之導電膏，且以漿料狀之狀態塗佈於連接對象構件上。
作為設置於上述連接對象構件之電極，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軟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積層鋁層而成之電極。作為上述金屬氧化物層之材料，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之導通材料。存在如下方法等：將導電性粒子混合於熱硬化性樹脂或熱UV併用硬化性樹脂中並進行分散，點狀塗佈於單側基板上並與對向基板貼合的方法；以及將導電性粒子混合於周邊密封劑中並進行分散，線狀地塗佈，兼用密封與上下基板之電性連接的方法等。於上述使用形態中亦可應用本發明之導電性粒子。
以下，列舉實施例及比較例對本發明具體地進行說明。本發明並不僅限於以下之實施例。
以下之實施例所使用之導電材之粉體電阻率顯示0.1Ω‧cm以下之值。關於導電材之粉體電阻率，具體而言，為鉬(Mo)(0.001Ω‧cm)、鎢(W)(0.001Ω‧cm)、碳化鎢(WC)(0.005Ω‧cm)、碳化鈦(TiC)(0.005Ω‧cm)、碳化鉭(TaC)(0.003Ω‧cm)。
上述粉體電阻率係利用三菱化學公司製造之製粉體電阻率測定系統「Loresta GP」，使用導電材2.5g，以23℃下荷重20kN時之粉體電阻率求出。
(實施例1)
(1)鈀附著步驟
準備粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-205」)。對該樹脂粒子進行蝕刻並進行水洗。繼而，於含有鈀觸媒8重量%之鈀觸媒化液100mL中添加樹脂粒子，進行攪拌。其後，進行過濾並進行清洗。於pH值6之0.5重量%二甲胺硼 烷液中添加樹脂粒子，而獲得附著有鈀之樹脂粒子。
(2)導電材附著步驟
將附著有鈀之樹脂粒子於離子交換水400mL中攪拌3分鐘，使之分散而獲得分散液。繼而，歷時3分鐘將含有碳化鎢粒子(平均粒徑100nm)5重量%之漿料400g添加於獲得之分散液中，獲得含有附著有導電材之樹脂粒子之懸浮液。
(3)無電鍍鎳步驟
準備含有硫酸鎳0.23mol/L、二甲胺硼烷0.92mol/L、及檸檬酸鈉0.5mol/L之鎳鍍液(pH值8.5)。
一面於60℃下攪拌所獲得之懸浮液，一面將上述鎳鍍液緩慢地滴加至懸浮液而進行無電鍍鎳。其後，藉由將懸浮液過濾而取出粒子，進行水洗並進行乾燥，藉此獲得於附著有導電材之樹脂粒子之表面上配置有鎳層(厚度0.1μm)之導電性粒子。鎳層100重量%中，鎳之含量為98.9重量%，硼之含量為1.1重量%。所獲得之導電性粒子具備埋入導電層內之複數之導電材，於導電層之外側之表面具有複數個突起，且於導電層之突起之內側配置有導電材。
(實施例2)
將碳化鎢粒子(平均粒徑100nm)變更為鎢粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(實施例3)
將碳化鎢粒子(平均粒徑100nm)變更為碳化鉭粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(實施例4)
將碳化鎢粒子(平均粒徑100nm)變更為鉬粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(實施例5)
(1)絕緣性粒子之製作
向安裝有4口可分離式蓋、攪拌葉、三向旋塞、冷卻管及溫度探針之1000mL之可分離式燒瓶中，將含有甲基丙烯酸甲酯100mmol、N,N,N-三甲基-N-2-甲基丙烯醯氧基乙基氯化胺1mmol、及2,2'-偶氮雙(2-脒基丙烷)二鹽酸鹽1mmol之單體組合物以固形物成分率成為5重量%的方式稱取至離子交換水中後，以200rpm進行攪拌，於氮氣環境下以70℃進行聚合24小時。反應結束後，進行冷凍乾燥，而獲得於表面具有銨基、且平均粒徑220nm及CV值10%之絕緣性粒子。
(2)絕緣性粒子之附著步驟
於超音波照射下使絕緣性粒子分散於離子交換水中，而獲得絕緣性粒子之10重量%水分散液。
使實施例1中獲得之導電性粒子10g分散於離子交換水500mL中，添加絕緣性粒子之水分散液4g，於室溫下攪拌6小時。利用3μm之篩網過濾器進行過濾後，進而利用甲醇進行清洗，進行乾燥而獲得附著有絕緣性粒子之導電性粒子。
利用掃描式電子顯微鏡(SEM)進行觀察，結果，於導電性粒子之表面僅形成有1層絕緣性粒子之被覆層。根據圖像解析，算出絕緣性粒子對於距導電性粒子中心2.5μm處之面積的被覆面積(即，絕緣性粒子之粒徑之投影面積)，結果被覆率為35%。
(實施例6)
將使絕緣性粒子附著前之實施例1中獲得之導電性粒子變更為實施例2中獲得之導電性粒子，除此以外，以與實施例5相同之方式獲得導電性粒子。
(實施例7)
將使絕緣性粒子附著前之實施例1中獲得之導電性粒子變更為實施例3中獲得之導電性粒子，除此以外，以與實施例5相同之方式獲得 導電性粒子。
(實施例8)
將使絕緣性粒子附著前之實施例1中獲得之導電性粒子變更為實施例4中獲得之導電性粒子，除此以外，以與實施例5相同之方式獲得導電性粒子。
(實施例9)
將實施例1中獲得之導電性粒子10g添加於離子交換水500mL中，利用超音波處理機使之充分地分散，而獲得懸浮液。將該懸浮液於50℃下進行攪拌，並且準備含有硫酸鈀0.02mol/L、作為錯合劑之乙二胺0.04mol/L、作為還原劑之甲酸鈉0.06mol/L及結晶調整劑的pH值10.0之無電電鍍液。
於所獲得之懸浮液中緩慢地添加上述無電電鍍液，而進行無電鍍鈀。於鈀層之厚度成為0.03μm之時間點上結束無電鍍鈀。繼而，進行清洗，並進行真空乾燥，藉此獲得於鎳層之表面積層有鈀層(厚度0.03μm)之導電性粒子。
(實施例10)
將形成鈀層前之實施例1中獲得之導電性粒子變更為實施例2中獲得之導電性粒子，除此以外，以與實施例9相同之方式獲得導電性粒子。
(實施例11)
將形成鈀層前之實施例1中獲得之導電性粒子變更為實施例3中獲得之導電性粒子，除此以外，以與實施例9相同之方式獲得導電性粒子。
(實施例12)
將形成鈀層前之實施例1中獲得之導電性粒子變更為實施例4中獲得之導電性粒子，除此以外，以與實施例9相同之方式獲得導電性 粒子。
(實施例13)
將粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)變更為粒徑為2.5μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-2025」)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(實施例14)
(1)鈀附著步驟
準備粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)。對該樹脂粒子進行蝕刻，並進行水洗。繼而，於含有鈀觸媒8重量%之鈀觸媒化液100mL中添加樹脂粒子並進行攪拌。其後，進行過濾並進行清洗。於pH值6之0.5重量%二甲胺硼烷液中添加樹脂粒子，獲得附著有鈀之樹脂粒子。
(2)導電材附著步驟
將附著有鈀之樹脂粒子於離子交換水400mL中攪拌3分鐘，使之分散而獲得分散液。繼而，歷時3分鐘將含有碳化鎢粒子(平均粒徑100nm)5重量%之漿料400g添加於所獲得之分散液中，獲得含有附著有導電材之樹脂粒子之懸浮液。
(3)無電鍍鎳步驟
準備含有硫酸鎳0.25mol/L、次亞磷酸鈉0.25mol/L及檸檬酸鈉0.15mol/L之鎳鍍液(pH值9.0)。
將所獲得之懸浮液於70℃下進行攪拌，並且將上述鎳鍍液緩慢地滴加於懸浮液而進行無電鍍鎳。其後，藉由將懸浮液過濾而取出粒子，進行水洗並進行乾燥，藉此獲得於樹脂粒子之表面配置有鎳-磷導電層(厚度0.1μm)之導電性粒子。
(實施例15)
(1)鈀附著步驟
準備粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)。對該樹脂粒子進行蝕刻，並進行水洗。繼而，於含有鈀觸媒8重量%之鈀觸媒化液100mL中添加樹脂粒子並進行攪拌。其後，進行過濾並進行清洗。於pH值6之0.5重量%二甲胺硼烷液中添加樹脂粒子，獲得附著有鈀之樹脂粒子。
(2)導電材附著步驟
將附著有鈀之樹脂粒子於離子交換水400mL中攪拌3分鐘，使之分散而獲得分散液。繼而，歷時3分鐘將含有碳化鎢粒子(平均粒徑100nm)5重量%之漿料400g添加於所獲得之分散液中，獲得含有附著有導電材之樹脂粒子之懸浮液。
(3)無電鍍鎳步驟
準備含有硫酸鎳0.25mol/L、次亞磷酸鈉0.25mol/L及檸檬酸鈉0.15mol/L之鎳鍍液(pH值6.0)。
將獲得之懸浮液於60℃下進行攪拌，並且將上述鎳鍍液緩慢地滴加於懸浮液而進行無電鍍鎳。繼而，將含有硫酸鎳0.25mol/L、次亞磷酸鈉0.25mol/L及檸檬酸鈉0.15mol/L之鎳鍍液(pH值10.0)緩慢地滴加於懸浮液，而進行無電鍍鎳。其後，藉由將懸浮液過濾而取出粒子，進行水洗並進行乾燥，藉此獲得於樹脂粒子之表面配置有鎳-磷導電層(厚度0.1μm)之導電性粒子。
(實施例16)
(1)鈀附著步驟
準備粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)。對該樹脂粒子進行蝕刻，並進行水洗。繼而，於含有鈀觸媒8重量%之鈀觸媒化液100mL中添加樹脂粒子並進行攪拌。其後，進行過濾並進行清洗。於pH值6之0.5重量%二甲胺硼 烷液中添加樹脂粒子，而獲得附著有鈀之樹脂粒子。
(2)導電材附著步驟
將附著有鈀之樹脂粒子於離子交換水400mL中攪拌3分鐘，使之分散而獲得分散液。繼而，歷時3分鐘將含有碳化鎢粒子(平均粒徑100nm)5重量%之漿料400g添加於獲得之分散液中，獲得含有附著有導電材之樹脂粒子之懸浮液。
(3)無電鍍鎳步驟
準備含有硫酸鎳0.23mol/L、二甲胺硼烷0.92mol/L、檸檬酸鈉0.5mol/L及鎢酸鈉0.01mol/L之鎳鍍液(pH值8.5)。
將所獲得之懸浮液於60℃下進行攪拌，並且將上述鎳鍍液緩慢地滴加於懸浮液而進行無電鍍鎳。其後，藉由將懸浮液過濾而取出粒子，進行水洗並進行乾燥，藉此獲得於樹脂粒子之表面設置有鎳-鎢-硼導電層(厚度約0.1μm)之導電性粒子。
(參考例1)
將碳化鎢粒子(平均粒徑100nm)變更為鎳粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(比較例1)
將碳化鎢粒子(平均粒徑100nm)變更為銅粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(比較例2)
將碳化鎢粒子(平均粒徑100nm)變更為二氧化矽粒子(平均粒徑100nm)，除此以外，以與實施例1相同之方式獲得導電性粒子。
(實施例17)
(1)鈀附著步驟
準備粒徑為3.0μm之二乙烯苯樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)。對該樹脂粒子進行蝕刻，並進行水洗。繼 而，於含有鈀觸媒8重量%之鈀觸媒化液100mL中添加樹脂粒子並進行攪拌。其後，進行過濾並進行清洗。於pH值6之0.5重量%二甲胺硼烷液中添加樹脂粒子，獲得附著有鈀之樹脂粒子。
(2)導電材附著步驟
將附著有鈀之樹脂粒子於離子交換水400mL中攪拌3分鐘，使之分散而獲得分散液。繼而，歷時3分鐘將含有碳化鎢粒子(平均粒徑100nm)5重量%之漿料400g添加於獲得之分散液中，獲得含有附著有導電材之樹脂粒子之懸浮液。
(3)無電鍍銅步驟
準備含有硫酸銅0.23mol/L、乙二胺四乙酸鹽2.3mol/L、福馬林0.5mol/L之鍍銅液(pH值12.5)。將所獲得之懸浮液於60℃下進行攪拌，並且將上述鍍銅液緩慢地滴加於懸浮液而進行無電鍍銅。其後，藉由將懸浮液過濾而取出粒子，進行水洗並進行乾燥，藉此獲得於樹脂粒子之表面上配置有銅導電層(厚度0.1μm)之導電性粒子。
(評價)
(1)連接電阻
連接構造體之製作：
將雙酚A型環氧樹脂(三菱化學公司製造之「Epikote 1009」)10重量份、丙烯酸系橡膠(重量平均分子量約80萬)40重量份、甲基乙基酮200重量份、微膠囊型硬化劑(旭化成化學公司製造之「HX3941HP」)50重量份、及矽烷偶合劑(Dow Corning Toray Silicone公司製造之「SH6040」)2重量份進行混合，將導電性粒子以含量成為3重量%之方式進行添加，並使該導電性粒子分散，而獲得樹脂組合物。
將所獲得之樹脂組合物塗佈於單面經脫模處理之厚度50μm之PET(聚對苯二甲酸乙二酯)膜上，利用70℃之熱風進行5分鐘乾燥，而 製作各向異性導電膜。所獲得之各向異性導電膜之厚度為12μm。
將所獲得之各向異性導電膜切割成5mm×5mm之尺寸。將切割而成之各向異性導電膜貼附於一面具有擁有電阻測定用之引繞線之鋁電極(高度0.2μm、L/S=20μm/20μm)之玻璃基板(寬3cm、長3cm)的鋁電極側之大致中央。繼而，將具有相同鋁電極之2層軟性印刷基板(寬2cm、長1cm)以電極彼此重疊之方式進行位置對準後進行貼合。將該玻璃基板與2層軟性印刷基板之積層體於10N、180℃、及20秒鐘之壓接條件下進行熱壓接，而獲得連接構造體。再者，使用在聚醯亞胺膜上直接形成有鋁電極之2層軟性印刷基板。
連接電阻之測定：
利用4端子法測定所獲得之連接構造體之對向之電極間的連接電阻。又，利用下述基準判定連接電阻。
[連接電阻之評價基準]
￮￮：未達使用參考例1之導電性粒子之情形之連接電阻的90%
￮：為使用參考例1之導電性粒子之情形之連接電阻的90%以上且未達95%
△：為使用參考例1之導電性粒子之情形之連接電阻的95%以上且未達105%
×：為使用參考例1之導電性粒子之情形之連接電阻的105%以上
將結果示於下述之表1、2。
1‧‧‧導電性粒子
1a‧‧‧突起
2‧‧‧基材粒子
3‧‧‧導電層
3a‧‧‧突起
4‧‧‧導電材
5‧‧‧絕緣性物質

Claims (9)

  1. 一種導電性粒子，其具備：基材粒子、配置於上述基材粒子之表面上之導電層、與配置於上述基材粒子之表面上之一部分區域的導電材，上述導電材被埋入上述導電層內，且上述導電材之材質為鉬、碳化鎢、鎢、碳化鈦或碳化鉭。
  2. 如請求項1之導電性粒子，其具備複數之上述導電材。
  3. 如請求項1或2之導電性粒子，其中上述導電層於外側之表面具有突起，且於上述導電層之上述突起之內側配置有上述導電材。
  4. 如請求項1或2之導電性粒子，其中上述導電層具有鎳層。
  5. 如請求項1或2之導電性粒子，其中上述導電層於上述基材粒子側具有鎳層，於與上述基材粒子側相反側具有鈀層。
  6. 如請求項1或2之導電性粒子，其進而具備附著於上述導電層之表面之絕緣性物質。
  7. 如請求項1或2之導電性粒子，其中上述導電材為粒子。
  8. 一種導電材料，其含有如請求項1至7中任一項之導電性粒子與黏合劑樹脂。
  9. 一種連接構造體，其具備：於表面具有第1電極之第1連接對象構件、於表面具有第2電極之第2連接對象構件、及將上述第1連接對象構件與上述第2連接對象構件連接之連接部，且上述連接部由如請求項1至7中任一項之導電性粒子形成，或 者由含有上述導電性粒子與黏合劑樹脂之導電材料形成，且上述第1電極與上述第2電極由上述導電性粒子電性連接。
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