CN110000372A - 导电性粒子、导电材料及连接结构体 - Google Patents

导电性粒子、导电材料及连接结构体 Download PDF

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Publication number
CN110000372A
CN110000372A CN201910187736.7A CN201910187736A CN110000372A CN 110000372 A CN110000372 A CN 110000372A CN 201910187736 A CN201910187736 A CN 201910187736A CN 110000372 A CN110000372 A CN 110000372A
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particle
mentioned
electroconductive particle
conductive layer
conductive
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CN201910187736.7A
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西冈敬三
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Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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    • 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
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    • 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
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Abstract

本发明提供一种在对电极间进行了连接的情况下可以使连接电阻降低的导电性粒子、以及使用了该导电性粒子的导电材料。本发明的导电性粒子1具备基体材料粒子2、以及在基体材料粒子2的表面上的一部分区域配置的导电材料4，且导电材料4的材质为莫氏硬度高于镍的材质。

Description

导电性粒子、导电材料及连接结构体
本申请是中国申请号为201380037610.2，申请日为2013年9月30日，发明名称为“导电性粒子、导电材料及连接结构体”的中国发明专利申请的分案申请。
技术领域
本发明涉及在基体材料粒子的表面上配置导电材料而成的导电性粒子。更详细而言，本发明例如涉及可用于电极间的电连接的导电性粒子。另外，本发明涉及使用上述导电性粒子的导电材料及连接结构体。
背景技术
各向异性导电膏及各向异性导电膜等导电材料已广为人知。这些各向异性导电材料中，在粘合剂树脂中分散有导电性粒子。
为了获得各种连接结构体，上述各向异性导电材料例如被用于挠性印制基板与玻璃基板的连接(FOG(Film on Glass))、半导体芯片与挠性印制基板的连接(COF(Chip onFilm))、半导体芯片与玻璃基板的连接(COG(Chip on Glass))、以及挠性印制基板与环氧玻璃基板的连接(FOB(Film on Board))等。
作为上述导电性粒子的一例，下述专利文献1中公开有具备复合粒子以及覆盖该复合粒子的金属镀层的导电性粒子。上述复合粒子具有塑料核体、以及通过化学键合而吸附于该塑料核体的非导电性无机粒子。
下述专利文献2中公开有如下导电性粒子，其具备塑料核体、覆盖该塑料核体的高分子电解质层、隔着该高分子电解质层而吸附于上述塑料核体的金属粒子、及在上述塑料核体周围形成的非电镀金属层而覆盖该金属粒子。专利文献2中记载有吸附于上述塑料核体的金属粒子为例如选自金、银、铜、钯及镍中的金属的粒子。
下述专利文献3中公开有如下导电性粒子，在基体材料粒子的表面形成有含有镍及磷的金属镀敷被膜层和金层形成的多层导电层。该导电性粒子中，在基体材料粒子的表面上配置有芯物质，且该芯物质被导电层包覆。导电层因芯物质而隆起，从而导电层的表面形成有突起。专利文献3中，在构成上述芯物质的导电性物质为金属的情况下，作为该金属，例如可举出：镍、铜、金、银、铂、锌、铁、铅、锡、铝、钴、铟、铬、钛、锑、铋、锗及镉等金属、以及锡-铅合金、锡-铜合金、锡-银合金及锡-铅-银合金等由2种以上金属构成的合金等。
现有技术文献
专利文献
专利文献1：日本专利特开2011-29179号公报
专利文献2：日本专利特开2011-108446号公报
专利文献3：日本专利特开2006-228475号公报
发明内容
发明要解决的问题
上述专利文献1～3中公开了在导电层的外侧表面具有突起的导电性粒子。多数情况下，在由导电性粒子进行连接的电极、及导电性粒子的导电层的表面形成有氧化被膜。上述导电层的突起为了在隔着导电性粒子对电极间进行压接时，除去电极及导电性粒子表面的氧化被膜并使导电层与电极接触而形成。
但是，在使用如专利文献1～3所记载的现有的导电性粒子而对电极间进行连接的情况下，有时连接电阻提高。另外，不能充分地除去电极及导电性粒子表面的氧化被膜，从而连接电阻容易变得较高。
另外，近年来，期待一种可使电极间的连接电阻进一步降低的导电性粒子。
本发明的目的在于，提供一种在将电极间连接的情况下可使电极间的连接电阻降低的导电性粒子、以及使用该导电性粒子的导电材料及连接结构体。
解决问题的方法
根据本发明的大的方面，提供一种导电性粒子，其具有：基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的导电材料，所述导电材料的材质为莫氏硬度高于镍的材质。
本发明的导电性粒子的某特定方面中，所述导电性粒子具备：所述基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，所述导电材料的材质为钼、碳化钨、钨、碳化钛或碳化钽。
本发明的导电性粒子的某特定方面中，该导电性粒子具有多个所述导电材料。
本发明的导电性粒子的某特定方面中，该导电性粒子具备：所述基体材料粒子、配置于所述基体材料粒子表面上的导电层、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，所述导电材料被埋入所述导电层内。
本发明的导电性粒子的某特定方面中，所述导电层在外侧表面具有突起，且在所述导电层的所述突起的内侧配置有所述导电材料。
本发明的导电性粒子的某特定方面中，所述导电层具有镍层。
本发明的导电性粒子的某特定方面中，所述导电层在所述基体材料粒子侧具有镍层，在与所述基体材料粒子侧相反的一侧具有钯层。
本发明的导电性粒子的某特定方面中，该导电性粒子还具有附着于所述导电层表面的绝缘性物质。
本发明的导电性粒子的某特定方面中，所述导电材料为粒子。
本发明的导电性粒子的某特定方面中，所述导电性粒子具备所述基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，所述导电材料的材质为钼、碳化钨、钨或碳化钽。
根据本发明的大的方面，提供一种导电材料，其含有所述的导电性粒子和粘合剂树脂。
根据本发明的大的方面，提供一种连接结构体，其具备：在表面具有第1电极的第1连接对象部件、在表面具有第2电极的第2连接对象部件、将所述第1连接对象部件和所述第2连接对象部件连接的连接部，所述连接部由上述的导电性粒子形成，或由含有所述导电性粒子和粘合剂树脂的导电材料形成，所述第1电极和所述第2电极通过所述导电性粒子实现了电连接。
发明效果
本发明的导电性粒子在基体材料粒子表面上的部分区域配置有导电材料，且上述导电材料的材质为莫氏硬度高于镍的材质，因此，在使用本发明的导电性粒子对电极间进行连接的情况下，可使连接电阻降低。
附图说明
图1是表示本发明的第1实施方式的导电性粒子的剖面图。
图2是表示本发明的第2实施方式的导电性粒子的剖面图。
图3是表示本发明的第3实施方式的导电性粒子的剖面图。
图4是示意性地表示使用本发明的第1实施方式的导电性粒子的连接结构体的正面剖面图。
标记说明
1 导电性粒子
1a 突起
2 基体材料粒子
3 导电层
3a 突起
4 导电材料
5 绝缘性物质
11 导电性粒子
11a 突起
12 第1导电层
13 第2导电层
13a 突起
21 导电性粒子
22 导电层
51 连接结构体
52 第1连接对象部件
52a 第1电极
53 第2连接对象部件
53a 第2电极
54 连接部
具体实施方式
以下，对本发明的详细内容进行说明。
(导电性粒子)
本发明的导电性粒子具备：基体材料粒子、以及配置在该基体材料粒子表面的部分区域的导电材料。上述导电材料的材质为莫氏硬度高于镍的材质。
通过采用本发明的导电性粒子的上述结构，在使用本发明的导电性粒子对电极间进行连接的情况下，不易产生电极间的连接不良，进而可有效地降低电极间的连接电阻。
上述导电材料的材质优选为钼、钨、碳化钨、碳化钛或碳化钽，也优选为钼、钨、碳化钨、或碳化钽。这些材质的莫氏硬度较高。在使用具备这些材质的导电材料的导电性粒子对电极间进行连接的情况下，不易产生电极间的连接不良，进而可有效地降低电极间的连接电阻。
本发明的导电性粒子优选为具备：上述基体材料粒子、配置在上述基体材料粒子表面上的导电层、及配置在上述基体材料粒子表面上的部分区域的上述导电材料。该情况下，上述导电材料优选为被埋入上述导电层内。上述导电层的部分区域优选为与上述基体材料粒子接触。
通过使用将上述导电材料埋入到上述导电层内的导电性粒子，在使用导电性粒子对电极间进行连接的情况下，更加不易产生电极间的连接不良，进而可进一步降低电极间的连接电阻。
就本发明的导电性粒子而言，优选为上述导电层在外侧的表面具有突起，且在上述导电层的上述突起的内侧配置有上述导电材料。优选为由上述导电材料形成上述突起。
多数情况下，在由导电性粒子连接的电极的表面形成有氧化被膜。另外，多数情况下，在上述导电层的外侧表面形成有氧化被膜。基于上述导电层在外侧表面具有多个突起，在电极间配置导电性粒子，然后进行压接，由此利用突起去除氧化被膜。因此，可使电极与导电性粒子进一步可靠地接触，可进一步降低电极间的连接电阻。
以下，参照附图对本发明的具体实施方式及实施例进行说明，由此明确本发明。
图1是表示本发明的第1实施方式的导电性粒子的剖面图。
图1所示的导电性粒子1具备：基体材料粒子2、导电层3、多个导电材料4、以及多个绝缘性物质5。导电层3配置在基体材料粒子2的表面上。导电性粒子1中，形成有单层的导电层3。导电层3包覆有基体材料粒子2。导电层3还包覆有导电材料4。导电层3在外侧的表面具有多个突起3a。
导电性粒子1具备多个导电材料4。多个导电材料4被配置在基体材料粒子2表面上的部分区域，且埋入导电层3内。导电材料4未被配置在基体材料粒子2的表面上的全部区域。导电材料4未配置于基体材料粒子2的整个表面。导电材料4被配置在基体材料粒子2表面上的部分区域，因此，基体材料粒子2具有不与导电材料4接触的表面区域。导电材料4配置在突起3a的内侧。在1个突起3a的内侧配置有1个导电材料4。导电层3的外侧的表面因多个导电材料4而隆起，形成多个突起3a。导电性粒子具备多个导电材料，由此，容易在导电性粒子的外侧表面形成多个突起。
导电材料4为粒子。由于导电材料4为粒子，因此在基体材料粒子2表面上的部分区域配置有导电材料4。
导电材料4与基体材料粒子2接触。也可以在基体材料粒子表面与导电材料表面之间配置有导电层。还可以为基体材料粒子的表面与导电材料的表面之间隔开距离从而导电材料不与基体材料粒子接触。
绝缘性物质5配置在导电层3的表面上。绝缘性物质5为绝缘性粒子。绝缘性物质5由具有绝缘性的材料形成。导电性粒子未必一定具备绝缘性物质。另外，导电性粒子除具备绝缘粒子作为绝缘性物质外，也可以具备对导电层的外侧表面进行包覆的绝缘层作为绝缘性物质。
图2是表示本发明的第2实施方式的导电性粒子的剖面图。
图2所示的导电性粒子11具备：基体材料粒子2、第一导电层12、第二导电层13、多个导电材料4、及多个绝缘性物质5。
就导电性粒子1和导电性粒子11而言，仅导电层不同。即，导电性粒子1形成有1层结构的导电层，与之相对，导电性粒子11形成有两层结构的第一导电层12及第二导电层13。导电材料4被埋入第一导电层11及导电层13内。
第一导电层12配置在基体材料粒子2的表面上。在基体材料粒子2与第二导电层13之间配置有第一导电层12。第一导电层12为位于基体材料粒子2侧、且与基体材料粒子2相接触的导电层。第二导电层13位于与基体材料粒子2侧相反的一侧，且不与基体材料粒子2接触。因此，在基体材料粒子2的表面上配置有第一导电层12，在第一导电层12的表面上配置有第二导电层13。在第二导电层13的外表面具有多个突起13a。导电性粒子11在导电性的表面具有多个突起11a。
图3是表示本发明的第3实施方式的导电性粒子的剖面图。
图3所示的导电性粒子21具备：基体材料粒子2、导电层22、及多个导电材料4。导电层22配置在基体材料粒子2的表面上。导电材料4被埋入导电层22内。
导电性粒子21在表面不具有突起。导电性粒子21为球状。导电层22在外侧的表面不具有突起。如上所述，本发明的导电性粒子也可不具有突起，还也可为球状。另外，导电性粒子21不具有绝缘性物质。但是，导电性粒子21也可以具备配置在导电层22的表面上的绝缘性物质。
以下，更详细地对导电性粒子进行说明。
[基体材料粒子]
作为上述基体材料粒子，可举出：树脂粒子、除金属粒子以外的无机粒子、有机无机杂化粒子及金属粒子等。其中，优选除金属粒子之外的基体材料粒子，更优选树脂粒子、除金属粒子之外的无机粒子或有机无机杂化粒子。
作为用于形成上述树脂粒子的树脂，可适宜使用各种有机物。作为用于形成上述树脂粒子的树脂，例如可举出：聚乙烯、聚丙烯、聚苯乙烯、聚氯乙烯、聚偏氯乙烯、聚异丁烯、聚丁二烯等聚烯烃树脂；聚甲基丙烯酸甲酯及聚丙烯酸甲酯等丙烯酸类树脂；聚对苯二甲酸亚烷基二醇酯、聚碳酸酯、聚酰胺、苯酚甲醛树酯、三聚氰胺甲醛树脂、苯并胍胺甲醛树脂、尿素甲醛树脂、酚醛树脂、三聚氰胺树脂、苯并胍胺树脂、尿素树脂、环氧树脂、不饱和聚酯树脂、饱和聚酯树脂、聚对苯二甲酸乙二醇酯、聚砜、聚苯醚、聚缩醛、聚酰亚胺、聚酰胺酰亚胺、聚醚醚酮、聚醚砜、二乙烯基苯聚合物、以及二乙烯基苯类共聚物等。作为上述二乙烯基苯类共聚物等，可举出：二乙烯基苯-苯乙烯共聚物及二乙烯基苯-(甲基)丙烯酸酯共聚物等。上述树脂粒子的硬度可容易地控制在适宜范围内，因此，用于形成上述树脂粒子的树脂优选为使1种或2种以上具有烯属不饱和基的聚合性单体发生聚合而成的聚合物。
在使具有烯属不饱和基的单体发生聚合而获得上述树脂粒子的情况下，作为该具有烯属不饱和基的单体，可举出非交联性的单体及交联性的单体。
作为上述非交联性的单体，例如可举出：苯乙烯、α-甲基苯乙烯等苯乙烯类单体；(甲基)丙烯酸、马来酸、马来酸酐等含羧基单体；(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)丙烯酸硬脂酯、(甲基)丙烯酸环己酯、(甲基)丙烯酸异冰片酯等(甲基)丙烯酸烷基酯类；(甲基)丙烯酸2-羟基乙酯、(甲基)丙烯酸甘油酯、聚氧乙烯(甲基)丙烯酸酯、(甲基)丙烯酸缩水甘油酯等含有氧原子的(甲基)丙烯酸酯类；(甲基)丙烯腈等含腈单体；甲基乙烯基醚、乙基乙烯基醚、丙基乙烯基醚等乙烯基醚类；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类；乙烯、丙烯、异戊二烯、丁二烯等不饱和烃；(甲基)丙烯酸三氟甲酯、(甲基)丙烯酸五氟乙酯、氯乙烯、氟乙烯、氯苯乙烯等含卤素单体等。
作为上述交联性的单体，例如可举出：四羟甲基甲烷四(甲基)丙烯酸酯、四羟甲基甲烷三(甲基)丙烯酸酯、四羟甲基甲烷二(甲基)丙烯酸酯、三羟甲基丙烷三(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)四亚甲基二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯等多官能(甲基)丙烯酸酯类；(异)氰脲酸三烯丙酯、苯偏三酸三烯丙酯、二乙烯基苯、苯二甲酸二烯丙酯、二烯丙基丙烯酰胺、二烯丙基醚、γ-(甲基)丙烯酰氧基丙基三甲氧基硅烷、三甲氧基甲硅烷基苯乙烯、乙烯基三甲氧基硅烷等含硅烷单体等。
通过公知的方法对上述具有烯属不饱和基的聚合性单体进行聚合，可获得上述树脂粒子。作为该方法，例如可举出如下方法：在自由基聚合引发剂的存在下进行悬浮聚合的方法、以及使用非交联的种粒子与自由基聚合引发剂一起使单体溶胀而发生聚合的方法等。
在上述基体材料粒子为除金属以外的无机粒子或有机无机杂化粒子的情况下，作为用于形成基体材料粒子的无机物，可举出二氧化硅及炭黑等。作为由上述二氧化硅形成的粒子，没有特别限定，例如可举出对具有2个以上水解性烷氧基硅烷基的硅化合物进行水解而形成交联聚合物粒子，然后，根据需要进行烧制而获得的粒子。作为上述有机无机杂化粒子，例如可举出由进行了交联的烷氧基硅烷基聚合物与丙烯酸类树脂形成的有机无机杂化粒子等。
在上述基体材料粒子为金属粒子的情况下，作为用于形成该金属粒子的金属，可举出：银、铜、镍、硅、金及钛等。在上述基体材料粒子为金属粒子的情况下，该金属粒子优选为铜粒子。但是，上述基体材料粒子优选不是金属粒子。
上述基体材料粒子的粒径优选为0.1μm以上，更优选为1μm以上，进一步优选为1.5μm以上，特别优选为2μm以上，且优选为1000μm以下，更优选为500μm以下，进一步优选为300μm以下，进一步更优选为50μm以下，特别优选为30μm以下，最优选为5μm以下。若基体材料粒子的粒径为上述下限以上，则由于导电性粒子与电极的接触面积增大，因此，电极间的导通可靠性进一步提高，隔着导电性粒子进行了连接的电极间的连接电阻进一步降低。另外，通过非电解镀在基体材料粒子的表面形成导电层时，不易发生凝集，不易形成发生了凝集的导电性粒子。若粒径为上述上限以下，则导电性粒子容易被充分地压缩，电极间的连接电阻进一步降低，且电极间的间隔进一步变小。上述基体材料粒子的粒径在基体材料粒子为圆球状的情况下表示直径，在基体材料粒子并非圆球状的情况下表示最大直径。
上述基体材料粒子的粒径特别优选为2μm以上且5μm以下。若上述基体材料粒子的粒径为2～5μm的范围内，则电极间的间隔变小，并且即使导电层的厚度变厚，也可获得较小的导电性粒子。上述基体材料粒子的粒径也优选为3μm以下。
[导电层]
本发明的导电性粒子具有配置在基体材料粒子表面上的导电层。
用于形成上述导电层的金属没有特别限定。作为该金属，例如可举出：金、银、钯、铜、铂、锌、铁、锡、铅、铝、钴、铟、镍、铬、钛、锑、铋、铊、锗、镉、硅及它们的合金等。另外，作为上述金属，可举出锡掺杂氧化铟(ITO)及焊锡等。其中，可使电极间的连接电阻进一步降低，因此优选为含有锡的合金、镍、钯、铜或金，更优选为镍或钯。
如导电性粒子1、以及21，上述导电层可由1层形成。如导电性粒子11，导电层可由多层形成。即，导电层也可具有2层以上的叠层结构。在导电层由多层形成的情况下，最外层(第二导电层等)优选为金层、镍层、钯层、铜层或含有锡和银的合金层，更优选为钯层或金层。最外层优选为钯层，也优选为金层。在最外层为上述优选的导电层的情况下，电极间的连接电阻进一步降低。另外，在最外层为金层的情况下，耐腐蚀性进一步提高。镍层含有50重量％以上的镍。钯层或金层含有50重量％以上的钯或金。
与上述基体材料粒子接触的导电层优选为含有镍。在如导电性粒子1、以及21那样上述导电层为单层的情况下，上述导电层优选为含有镍。在如导电性粒子11那样导电层具有基体材料粒子侧的第一导电层以及与基体材料粒子侧相反的一侧的第二导电层的情况下，上述第一导电层(与基体材料粒子接触的导电层)优选为含有镍。上述导电层及上述第一导电层优选含有镍作为主成分。含有镍的导电层的导电性相对较高。因此，在通过具备含有镍的导电层的导电性粒子对电极间连接的情况下，电极间的连接电阻进一步降低。
与上述基体材料粒子接触的导电层100重量％中，镍的含量优选为50重量％以上。在上述导电层为单层的情况下，上述导电层100重量％中，镍的含量优选为50重量％以上。在上述导电层具备上述第1以及第二导电层的情况下，上述第一导电层100重量％中镍的含量优选为50重量％以上。若镍的含量为50重量％以上，则电极间的连接电阻充分降低。上述导电层或上述第一导电层100重量％中，镍的含量更优选为60重量％以上，进而优选为70重量％以上，特别优选为90重量％以上。上述导电层或上述第一导电层100重量％中镍的含量可为97重量％以上，可为97.5重量％以上，也可为98重量％以上。上述导电层或上述第一导电层100重量％中镍的含量优选为99.85重量％以下，更优选为99.7重量％以下，进一步优选为低于99.45重量％。若上述镍的含量为上述下限以上，则电极间的连接电阻进一步降低。另外，在电极或导电层表面的氧化被膜较少的情况下，具有上述镍的含量越多电极间的连接电阻越低的倾向。
上述导电层或上述第一导电层优选含有镍、并含有硼、磷中的至少1种。在上述导电层或上述第一导电层中，镍与选自硼、磷中的至少1种可进行合金化。另外，在上述导电层或上述第一导电层中，也可使用镍、硼以及磷以外的成分。
另外，连接结构体暴露在酸的存在下时，有时电极间的连接电阻上升。因此，有时上述导电层或上述第一导电层中，基体材料粒子侧的镍层中磷的含量较高、而与基体材料粒子相反一侧的镍层中磷的含量较低。
上述导电层或上述第一导电层100重量％中，硼和磷的总计含量优选为0.01重量％以上，更优选为0.05重量％以上，进而优选为0.1重量％以上，且优选为5重量％以下，更优选为4重量％以下，进而优选为3重量％以下，特别优选为2.5重量％以下，最优选为2重量％以下。若硼和磷的总计含量为上述下限以上，则上述导电层或上述第一导电层进一步变硬，可更有效地将电极及导电性粒子表面的氧化被膜去除，可使电极间的连接电阻进一步降低。若硼和磷的总计含量为上述上限以下，则镍的含量相对变多，因此，电极间的连接电阻降低。
上述导电层或上述第一导电层100重量％中，硼的含量优选为0.01重量％以上，更优选为0.05重量％以上，进一步优选为0.1重量％以上，且优选为5重量％以下，更优选为4重量％以下，进一步优选为3重量％以下，特别优选为2.5重量％以下，最优选为2重量％以下。若硼的含量为上述下限以上，则上述导电层或上述第一导电层进一步变硬，可更有效地将电极及导电性粒子表面的氧化被膜去除，从而可使电极间的连接电阻进一步降低。若硼的含量为上述上限以下，则镍的含量相对变多，因此，电极间的连接电阻降低。
上述导电层或上述第一导电层优选为不含磷，或者含有磷且上述导电层或上述第一导电层100重量％中磷的含量低于10.0重量％。上述导电层100重量％中，磷的含量更优选为低于0.5重量％，进而优选为0.3重量％以下，特别优选为0.1重量％以下。上述导电层或上述第一导电层特别优选为不含磷。
上述导电层或上述第一导电层中的镍、硼及磷等的各含量的测定方法可使用已知的各种分析法，没有特别限定。作为该测定方法，可举出吸光分析法或光谱分析法等。在上述吸光分析法中，可使用火焰吸光光度计及电加热炉吸光光度计等。作为上述光谱分析法，可举出等离子体发光分析法及等离子体离子源质谱分析法等。
对上述导电层或上述第一导电层中的镍、硼及磷等的各含量进行测定时，优选为使用ICP发光分析装置。作为ICP发光分析装置的市售品，可举出HORIBA社制的ICP发光分析装置等。
从使电极间的连接电阻进一步降低的观点出发，上述导电层优选在上述基体材料粒子侧具有镍层，在与上述基体材料粒子侧相反的一侧具有第二导电层。该情况下，第二导电层优选为钯层或金层，更优选为钯层，进而优选为金层。
在上述基体材料粒子的表面上形成上述导电层或上述第一导电层的方法、以及在上述第一导电层的表面上形成上述第二导电层的方法没有特别限定。作为形成导电层的方法，例如可举出：利用非电解镀的方法、利用电镀的方法、利用物理蒸镀的方法、以及将含有金属粉末或含有金属粉末和粘合剂的糊料涂布在基体材料粒子或其它导电层的表面的方法等。其中，因导电层的形成较为简单，所以优选为利用非电解镀的方法。作为上述利用物理蒸镀的方法，可举出真空蒸镀、离子镀及离子溅射等方法。
上述导电性粒子的粒径优选为0.5μm以上，更优选为1μm以上，且优选为100μm以下，更优选为20μm以下。若导电性粒子的粒径为上述下限以上及上限以下，则在使用导电性粒子对电极间进行连接的情况下，导电性粒子与电极的接触面积充分增大，从而在形成导电层时不易形成凝集的导电性粒子。另外，隔着导电性粒子所连接的电极间的间隔不会变得过大，且导电层不易从基体材料粒子的表面剥离。
上述导电性粒子的粒径在导电性粒子为圆球状的情况下表示直径，在导电性粒子不是圆球状的情况下表示最大直径。
导电性粒子的导电层整体的厚度、以及导电层为单层时的导电层的厚度优选为0.005μm以上，更优选为0.01μm以上，进一步优选为0.05μm以上，且优选为1μm以下，更优选为0.3μm以下。若上述导电层的厚度为上述下限以上及上述上限以下，则可获得充分的导电性，且导电性粒子不会变得过硬，从而在对电极间进行连接时导电性粒子发生充分地变形。
在导电层为2层以上的叠层结构的情况下，与基体材料粒子接触的导电层(第一导电层)的厚度优选为0.001μm以上，更优选为0.01μm以上，进一步优选为0.05μm以上，且优选为0.5μm以下，更优选为0.3μm以下，进一步优选为0.1μm以下。若与基体材料粒子接触的导电层的厚度为上述下限以上及上述上限以下，则可使导电层的包覆均匀，且电极间的连接电阻充分降低。
导电性粒子中的导电层整体的厚度、以及导电层为单层时的导电层的厚度特别优选为0.05μm以上且0.3μm以下。另外，特别优选基体材料粒子的粒径为2μm以上且5μm以下，且导电性粒子中的导电层整体的厚度、及导电层为单层时的导电层的厚度为0.05μm以上且0.3μm以下。该情况下，可适当地将导电性粒子用于通过较大电流的用途。另外，对导电性粒子进行压缩从而对电极间进行连接的情况下，可进一步抑制电极损伤。
上述导电层的厚度例如可使用透射式电子显微镜(TEM)对导电性粒子的剖面进行观察来测定。
作为对上述导电层以及上述第一导电层中的镍、硼及磷的含量进行控制的方法，例如可举出：在通过非电解镍电镀来形成导电层时，对镍镀液的pH值进行控制的方法；在通过非电解镍电镀来形成导电层时，对含硼的还原剂进行浓度调整的方法；在通过非电解镍电镀来形成导电层时，对含磷的还原剂进行浓度调整的方法；以及对镍镀液中的镍浓度进行调整的方法等。
在通过非电解镀形成的方法中，通常进行催化剂化工序和非电解镀工序。以下，对通过非电解镀而在树脂粒子的表面形成含有镍和硼的合金镀层的方法的一例进行说明。
上述催化剂化工序中，在树脂粒子的表面形成催化剂，所述催化剂为用于通过非电解镀来形成镀层的起点。
作为使上述催化剂形成于树脂粒子表面的方法，例如可举出：向含有氯化钯和氯化锡的溶液中添加树脂粒子，然后，利用酸溶液或碱溶液对树脂粒子表面进行活化，从而使钯在树脂粒子表面析出的方法；以及向含有硫酸钯和氨基吡啶的溶液中添加树脂粒子，然后，利用含有还原剂的溶液对树脂粒子的表面进行活化，而使钯在树脂粒子表面析出的方法等。可优选使用含硼的还原剂作为上述还原剂。另外，可通过使用含磷还原剂作为上述还原剂来形成含磷的导电层。
在上述非电解镀工序中，可优选使用含有含镍化合物及上述含硼还原剂的镍镀浴。通过将树脂粒子浸渍在镍镀浴中，可以使镍析出在表面上形成有催化剂的树脂粒子的表面上，从而可以形成含有镍和硼的导电层。
作为上述含镍化合物，可举出硫酸镍及氯化镍等。上述含镍化合物优选为镍盐。
作为上述含硼还原剂，可举出二甲基胺硼烷、硼氢化钠及硼氢化钾等。作为上述含磷还原剂，可举出次磷酸钠等。
[导电材料]
本发明的导电性粒子具备配置在基体材料粒子的表面上的导电材料。该导电材料的材质优选为钼(Mo)(莫氏硬度5.5)、钨(W)(莫氏硬度7.5)、碳化钨(WC)(莫氏硬度9)、碳化钛(TiC)(莫氏硬度9)、或碳化钽(TaC)(莫氏硬度9)。导电性粒子具备上述特定材质的导电材料，由此导电性粒子的导电性的表面充分变硬，从而可使电极间的连接电阻充分降低。上述导电材料的材质的莫氏硬度高于镍(Ni)(莫氏硬度5.0)的莫氏硬度。上述导电材料的材质优选为碳化钨或碳化钽。上述导电材料的材质优选为钼，优选为钨，优选为碳化钨，优选为碳化钛，优选为碳化钽。
上述导电材料的粉末电阻率的值优选为0.1Ω·cm以下。
本发明的导电性粒子优选在导电性的表面具有突起。上述导电层优选为在外侧的表面具有突起。该突起优选为多个。多数情况下，在由导电性粒子连接的电极的表面形成有氧化被膜。另外，多数情况下，在导电性粒子的导电层的表面形成有氧化被膜。通过使用具有突起的导电性粒子，在电极间配置了导电性粒子，然后，进行压接，由此利用突起有效地将氧化被膜去除。在上述突起的内侧存在特定材质的上述导电材料，由此变得容易利用突起充分地将氧化被膜去除。因此，可使电极与导电性粒子进一步可靠地接触，从而可使电极间的连接电阻降低。另外，在导电性粒子的表面具有绝缘性物质的情况下，或者导电性粒子被分散在粘合剂树脂中而用作导电材料的情况下，利用导电性粒子的突起，可有效地去除导电性粒子和电极之间的树脂。因此，可提高电极间的导通可靠性。
通过将上述导电材料埋入上述导电层中，容易使上述导电层在外侧的表面具有多个突起。
在上述导电性粒子具备上述导电层的情况下，上述导电材料可与上述基体材料粒子接触，也可不与上述基体材料粒子接触。也可在上述基体材料粒子和上述导电材料之间配置有上述导电层的一部分。
本发明的导电性粒子优选具备多个上述导电材料。该情况下，在导电层的内侧具有多个配置有上述导电材料的部位，可使导电性粒子的导电部变硬。另外，容易在导电性粒子及导电层的表面形成多个突起。
上述导电材料优选为粒子。该情况下，由于配置在导电层内侧的作为粒子的导电材料的形状，因而可有效地使导电性粒子的导电部变硬。另外，容易在导电性粒子及导电层的表面形成多个突起。
作为粒子的上述导电材料的形状优选为块状。关于作为粒子的上述导电材料，例如可举出：粒子状的块、多个微小粒子凝集而成的凝聚块、及不定形的块等。
将上述基体材料粒子的粒径设为D时，上述导电材料的最大直径优选为0.005D以上，更优选为0.015D以上，且优选为0.25D以下，更优选为0.15D以下。
另外，将上述基体材料粒子的粒径设为D时，上述导电层沿厚度方向上的上述导电材料的尺寸优选为0.005D以上，更优选为0.015D以上，且优选为0.25D以下，更优选为0.15D以下。
作为形成上述突起的方法，可举出：使上述导电材料附着在基体材料粒子的表面后利用非电解镀形成导电层的方法；以及利用非电解镀在基体材料粒子的表面形成了导电层后使上述导电材料附着，再利用非电解镀形成导电层的方法等。作为形成上述突起的其它方法，可举出：在基体材料粒子的表面上形成第一导电层后，在该第一导电层上配置上述导电材料，再形成第二导电层的方法；以及在基体材料粒子的表面上形成导电层的中途阶段添加上述导电材料的方法等。
每1个上述导电性粒子具有的上述导电材料的数量及上述突起的数量分别优选为3个以上，更优选为5个以上。上述导电材料的数量及上述突起的数量的上限没有特别限定。上述导电材料的数量及上述突起的数量的上限可考虑导电性粒子的粒径等来适当选择。
[绝缘性物质]
本发明的导电性粒子优选为具备在上述导电层的表面上所配置的绝缘性物质。该情况下，若将导电性粒子用于电极间的连接，则可进一步防止邻接的电极间的短路。具体而言，在多个导电性粒子发生接触时，在多个电极间存在绝缘性物质，因此，可防止横方向上相邻的电极间而非上下的电极间的短路。需要说明的是，在对电极间进行连接时，利用2个电极对导电性粒子进行加压，由此，可容易地将导电性粒子的导电层与电极之间的绝缘性物质去除。在导电性粒子中导电层的外侧表面具有多个突起的情况下，可容易地将导电性粒子的导电层与电极之间的绝缘性物质去除。
从对电极间进行压接时可更容易地将上述绝缘性物质去除出发，上述绝缘性物质优选为绝缘性粒子。
作为上述绝缘性物质的材料即绝缘性树脂的具体例，可举出：聚烯烃类、(甲基)丙烯酸酯聚合物、(甲基)丙烯酸酯共聚物、嵌段聚合物、热塑性树脂、热塑性树脂的交联物、热固化性树脂及水溶性树脂等。
(导电材料)
本发明的导电材料含有上述的导电性粒子以及粘合剂树脂。本发明的导电性粒子优选分散在粘合剂树脂中并用作导电材料。上述导电材料优选为各向异性导电材料。
上述粘合剂树脂没有特别限定。可使用公知的绝缘性的树脂作为上述粘合剂树脂。
作为上述粘合剂树脂，例如可举出：乙烯基树脂、热塑性树脂、固化性树脂、热塑性嵌段共聚物及弹性体等。上述粘合剂树脂可仅使用1种，也可组合使用2种以上。
作为上述乙烯基树脂，例如可举出：聚乙酸乙烯酯树脂、丙烯酸树脂及苯乙烯树脂等。作为上述热塑性树脂，例如可举出：聚烯烃树脂、乙烯-乙酸乙烯共聚物及聚酰胺树脂等。作为上述固化性树脂，例如可举出：环氧树脂、聚氨酯树脂、聚酰亚胺树脂及不饱和聚酯树脂等。需要说明的是，上述固化性树脂也可为常温固化型树脂、热固化型树脂、光固化型树脂或湿气固化型树脂。上述固化性树脂也可与固化剂组合使用。作为上述热塑性嵌段共聚物，例如可举出：苯乙烯-丁二烯-苯乙烯嵌段共聚物、苯乙烯-异戊二烯-苯乙烯嵌段共聚物、苯乙烯-丁二烯-苯乙烯嵌段共聚物的氢化物、以及苯乙烯-异戊二烯-苯乙烯嵌段共聚物的氢化物等。作为上述弹性体，例如可举出：苯乙烯-丁二烯共聚物橡胶、及丙烯腈-苯乙烯嵌段共聚物橡胶等。
上述导电材料除含有上述导电性粒子及上述粘合剂树脂外，例如还可以含有填充剂、增量剂、软化剂、增塑剂、聚合催化剂、固化催化剂、着色剂、抗氧化剂、热稳定剂、光稳定剂、紫外线吸收剂、润滑剂、抗静电剂及阻燃剂等各种添加剂。
使上述导电性粒子分散在上述粘合剂树脂中的方法可使用现有公知的分散方法，没有特别限定。作为使上述导电性粒子分散在上述粘合剂树脂中的方法，例如可举出：将上述导电性粒子添加到上述粘合剂树脂中，然后，利用行星混合机等进行混练而使其分散的方法；使用均质器等使上述导电性粒子均匀地分散在水或有机溶剂中，然后，添加到上述粘合剂树脂中，并利用行星混合机等进行混练而使其分散的方法；以及利用水或有机溶剂等对上述粘合剂树脂进行稀释后，添加上述导电性粒子，利用行星混合机等进行混练而使其分散的方法等。
本发明的导电材料可以以导电糊剂及导电膜等形式进行使用。本发明的导电材料为导电膜的情况下，可将不含导电性粒子的膜叠层在该含有导电性粒子的导电膜上。上述导电糊剂优选为各向异性导电糊剂。上述导电膜优选为各向异性导电膜。
上述导电材料100重量％中，上述粘合剂树脂的含量优选为10重量％以上，更优选为30重量％以上，进而优选为50重量％以上，特别优选为70重量％以上，且优选为99.99重量％以下，更优选为99.9重量％以下。若上述粘合剂树脂的含量为上述下限以上及上述上限以下，则导电性粒子被有效率地配置在电极间，由导电材料进行了连接的连接对象部件的连接可靠性进一步提高。
上述导电材料100重量％中，上述导电性粒子的含量优选为0.01重量％以上，更优选为0.1重量％以上，且优选为40重量％以下，更优选为20重量％以下，进而优选为10重量％以下。若上述导电性粒子的含量为上述下限以上及上述上限以下，则电极间的导通可靠性进一步提高。
(连接结构体)
使用本发明的导电性粒子、或者使用含有该导电性粒子以及粘合剂树脂的导电材料，通过对连接对象部件进行连接，可获得连接结构体。
上述连接结构体优选具备第1连接对象部件、第2连接对象部件、以及对第1连接对象部件及第2连接对象部件进行连接的连接部件，且该连接部由本发明的导电性粒子形成，或者由含有该导电性粒子以及粘合剂树脂的导电材料形成。在使用导电性粒子的情况下，连接部本身为导电性粒子。即，第1连接对象部件、第2连接对象部件通过导电性粒子被连接。
图4是示意性表示使用了本发明第1实施方式的导电性粒子的连接结构体的正面剖面图。
图4所示的连接结构体51具备第1连接对象部件52、第2连接对象部件53、及对第1连接对象部件52、第2连接对象部件53进行连接的连接部54。连接部54通过使含有导电性粒子1的导电材料固化而形成。需要说明的是，图4中，为图示方便，简略地对电性粒子1进行表示。
在第1连接对象部件52的表面(上表面)具有多个第1电极52a。在第2连接对象部件53的表面(下表面)具有多个第2电极53a。通过1个或多个导电性粒子1对第1电极52a以及第2电极53a进行电连接。因此，基于导电性粒子1对第1连接对象部件52、第2连接对象部件53进行电连接。
上述连接结构体的制造方法没有特别限定。作为连接结构体的制造方法的一例，可举出：在第1连接对象部件和第2连接对象部件之间配置上述导电材料而获得叠层体后，对该叠层体进行加热及加压的方法等。上述加压的压力为9.8×104～4.9×106Pa左右。上述加热的温度为120～220℃左右。
作为上述连接对象部件，具体而言，可举出：半导体晶片、电容器及二极管等电子部件、以及印制基板、挠性印制基板、环氧玻璃基板及玻璃基板等电路基板等电子部件等。上述导电材料优选为用于连接电子部件的导电材料。上述导电材料优选为浆料状的导电糊剂，且以糊状的状态涂布在连接对象部件上。
作为设置在上述连接对象部件的电极，可举出：金电极、镍电极、锡电极、铝电极、铜电极、钼电极及钨电极等金属电极。在上述连接对象部件为挠性印制基板的情况下，上述电极优选为金电极、镍电极、锡电极或铜电极。在上述连接对象部件为玻璃基板的情况下，上述电极优选为铝电极、铜电极、钼电极或钨电极。需要说明的是，在上述电极为铝电极的情况下，可为仅由铝形成的电极，也可为将铝层叠层在金属氧化物层的表面而成的电极。作为上述金属氧化物层的材料，可举出：掺杂有3价金属元素的氧化铟及掺杂有3价金属元素的氧化锌等。作为上述3价金属元素，可举出：Sn、Al及Ga等。
也可以列举本发明的导电性粒子的其它使用方式，即使用导电性粒子作为用于对构成液晶显示元件的上下基板间进行电连接的导通材料。还存在如下方法等：将导电性粒子混合到热固化性树脂或组合使用热UV的固化性树脂中并进行分散，在单侧基板上对其进行点状涂布并与对置的基板贴合的方法；以及将导电性粒子混合在周边密封剂中并使其分散，涂布为线状来兼顾密封以及上下基板的电连接的方法等。在上述使用方式中也可应用本发明的导电性粒子。
以下，列举实施例及比较例对本发明进行具体的说明。本发明并不仅限于以下的实施例。
以下的实施例中使用的导电材料的粉末电阻率显示0.1Ω·cm以下的值。关于导电材料的粉末电阻率，具体而言，为钼(Mo)(0.001Ω·cm)、钨(W)(0.001Ω·cm)、碳化钨(WC)(0.005Ω·cm)、碳化钛(TiC)(0.005Ω·cm)、碳化钽(TaC)(0.003Ω·cm)。
上述粉末电阻率利用三菱化学社制的粉末电阻率测定系统“Loresta GP”，使用导电材料2.5g，求出在23℃下荷重20kN时的粉末电阻率。
(实施例1)
(1)钯附着工序
准备粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制“Micropearl SP-205”)。对该树脂粒子进行浸湿并进行水洗。接着，将树脂粒子添加到含有钯催化剂8重量％的钯催化剂液100mL中，进行搅拌。然后，进行过滤并进行清洗。将树脂粒子添加到pH值为6的0.5重量％二甲基胺硼烷液中，从而获得附着有钯的树脂粒子。
(2)导电材料附着工序
将附着有钯的树脂粒子在离子交换水400mL中搅拌3分钟，使之分散而获得分散液。接着，将含有碳化钨粒子(平均粒径100nm)5重量％的浆料400g历时3分钟添加在获得的分散液中，获得含有附着有导电材料的树脂粒子的悬浮液。
(3)非电解镀镍工序
准备含有硫酸镍0.23mol/L、二甲基胺硼烷0.92mol/L、以及柠檬酸钠0.5mol/L的镀镍液(pH值8.5)。
在60℃下对所获得的悬浮液进行搅拌，同时，将上述镀镍溶液缓慢地滴加至悬浮液来进行非电解镀镍。其后，通过对悬浮液进行过滤而取出粒子，并进行水洗、干燥，由此获得在附着有导电材料的树脂粒子的表面上配置有镍层(厚度0.1μm)的导电性粒子。镍层100重量％中镍的含量为98.9重量％，硼的含量为1.1重量％。所获得的导电性粒子具备埋入导电层内的多个导电材料，在导电层的外侧表面具有多个突起，且在导电层的突起的内侧配置有导电材料。
(实施例2)
将碳化钨粒子(平均粒径100nm)变更为钨粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(实施例3)
将碳化钨粒子(平均粒径100nm)变更为碳化钽粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(实施例4)
将碳化钨粒子(平均粒径100nm)变更为钼粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(实施例5)
(1)绝缘性粒子的制作
向安装有4口可分离式盖、搅拌叶、三通阀、冷凝管及温度探针的1000mL的可分离式烧瓶中，将含有甲基丙烯酸甲酯100mmol、N,N,N-三甲基-N-2-甲基丙烯酰氧基乙基氯化铵1mmol、及2,2’-偶氮双(2-脒基丙烷)二盐酸盐1mmol的单体组合物称取至离子交换水中，使得固形物成分率成为5重量％，以200rpm进行搅拌，在氮气环境下以70℃进行聚合24小时。反应结束后，进行冷冻干燥，从而获得了在表面具有铵基，且平均粒径220nm及CV值10％的绝缘性粒子。
(2)绝缘性粒子的附着工序
在超声波照射下使绝缘性粒子分散在离子交换水中，获得了绝缘性粒子的10重量％水分散液。
使实施例1中获得的导电性粒子10g分散在离子交换水500mL中，添加绝缘性粒子的水分散液4g，在室温下搅拌6小时。利用3μm的筛网过滤器进行过滤后，进而利用甲醇进行清洗、干燥而获得附着有绝缘性粒子的导电性粒子。
利用扫描式电子显微镜(SEM)进行观察，结果，在导电性粒子的表面形成仅有1层绝缘性粒子的被覆层。通过图像解析，算出绝缘性粒子相对于距导电性粒子中心2.5μm处面积的被覆面积(即，绝缘性粒子的粒径的投影面积)，结果被覆率为35％。
(实施例6)
将使绝缘性粒子附着前的由实施例1获得的导电性粒子变更为实施例2中获得的导电性粒子，除此以外，与实施例5同样地获得导电性粒子。
(实施例7)
将使绝缘性粒子附着前的实施例1中获得的导电性粒子变更为实施例3中获得的导电性粒子，除此以外，与实施例5同样地获得导电性粒子。
(实施例8)
将使绝缘性粒子附着前的实施例1中获得的导电性粒子变更为实施例4中获得的导电性粒子，除此以外，与实施例5同样地获得导电性粒子。
(实施例9)
将实施例1中获得的导电性粒子10g添加在离子交换水500mL中，利用超声波处理机使其充分地分散，获得悬浮液。将该悬浮液在50℃下进行搅拌，并且准备pH值10.0的非电解镀溶液，所述非电解镀溶液含有硫酸钯0.02mol/L、作为络合剂的乙二胺0.04moUL、作为还原剂的甲酸钠0.06mol/L及结晶调整剂。
在所获得的悬浮液中缓慢地添加上述非电解镀液，进行非电解镀钯。在钯层的厚度成为0.03μm的时间点上结束非电解镀钯。接着，进行清洗，并进行真空干燥，由此获得在镍层表面叠层有钯层(厚度0.03μm)的导电性粒子。
(实施例10)
将形成钯层前的实施例1中获得的导电性粒子变更为实施例2中获得的导电性粒子，除此以外，与实施例9同样地获得导电性粒子。
(实施例11)
将形成钯层前的实施例1中获得的导电性粒子变更为实施例3中获得的导电性粒子，除此以外，与实施例9同样地获得导电性粒子。
(实施例12)
将形成钯层前的实施例1中获得的导电性粒子变更为实施例4中获得的导电性粒子，除此以外，与实施例9同样地获得导电性粒子。
(实施例13)
将粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-203”)变更为粒径为2.5μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-2025”)，除此以外，与实施例1同样地获得导电性粒子。
(实施例14)
(1)钯附着工序
准备粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-203”)。对该树脂粒子进行浸蚀，并进行水洗。接着，在含有钯催化剂8重量％的钯催化剂液100mL中添加树脂粒子并进行搅拌。其后，进行过滤并进行清洗。将树脂粒子添加至pH值6的0.5重量％二甲基胺硼烷液中来获得附着有钯的树脂粒子。
(2)导电材料附着工序
在离子交换水400mL中对附着有钯的树脂粒子搅拌3分钟，使之分散而获得分散液。接着，历时3分钟将含有碳化钨粒子(平均粒径100nm)5重量％的浆料400g添加在所获得的分散液中，从而获得含有附着有导电材料的树脂粒子的悬浮液。
(3)非电解镀镍工序
准备含有硫酸镍0.25mol/L、次磷酸钠0.25mol/L及柠檬酸钠0.15mol/L的镀镍溶液(pH值9.0)。
将所获得的悬浮液在70℃下进行搅拌，并且将上述镀镍液缓慢地滴加至悬浮液而进行非电解镀镍。其后，通过对悬浮液进行过滤而取出粒子，进行水洗并进行干燥，由此获得在树脂粒子的表面配置有镍-磷导电层(厚度0.1μm)的导电性粒子。
(实施例15)
(1)钯附着工序
准备粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-203”)。对该树脂粒子进行浸蚀，并进行水洗。接着，在含有钯催化剂8重量％的钯催化剂液100mL中添加树脂粒子并进行搅拌。其后，进行过滤并进行清洗。将树脂粒子添加在pH值6的0.5重量％二甲基胺硼烷液中，获得附着有钯的树脂粒子。
(2)导电材料附着工序
在离子交换水400mL中对附着有钯的树脂粒子搅拌3分钟，使之分散而获得分散液。接着，历时3分钟将含有碳化钨粒子(平均粒径100nm)5重量％的浆料400g添加在所获得的分散液中，从而获得含有附着有导电材料的树脂粒子的悬浮液。
(3)非电解镀镍工序
准备含有硫酸镍0.25mol/L、次磷酸钠0.25mol/L及柠檬酸钠0.15mol/L的镀镍液(pH值6.0)。
将获得的悬浮液在60℃下进行搅拌，并且将上述镀镍液缓慢地滴加至悬浮液而进行非电解镀镍。接着，将含有硫酸镍0.25mol/L、次磷酸钠0.25mol/L及柠檬酸钠0.15mol/L的镀镍液(pH值10.0)缓慢地滴加至悬浮液，进行非电解镀镍。其后，通过对悬浮液进行过滤而取出粒子，进行水洗并进行干燥，由此获得在树脂粒子的表面配置有镍-磷导电层(厚度0.1μm)的导电性粒子。
(实施例16)
(1)钯附着工序
准备粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-203”)。对该树脂粒子进行浸蚀，并进行水洗。接着，将树脂粒子添加至含有钯催化剂8重量％的钯催化剂液100mL中并进行搅拌。其后，进行过滤并进行清洗。将树脂粒子添加至pH值6的0.5重量％二甲胺硼烷溶液中，而获得附着有钯的树脂粒子。
(2)导电材料附着工序
在离子交换水400mL中对附着有钯的树脂粒子搅拌3分钟，使之分散而获得分散液。接着，历时3分钟将含有碳化钨粒子(平均粒径100nm)5重量％的浆料400g添加至获得的分散液中，从而获得含有附着有导电材料的树脂粒子的悬浮液。
(3)非电解镀镍工序
准备含有硫酸镍0.23mol/L、二甲基胺硼烷0.92mol/L、柠檬酸钠0.5mol/L及钨酸钠0.01mo1/L的镀镍液(pH值8.5)。
在60℃下对所获得的悬浮液进行搅拌，并且将上述镀镍溶液缓慢地滴加至悬浮液来进行非电解镀镍。其后，通过对悬浮液进行过滤而取出粒子，进行水洗并进行干燥，由此获得在树脂粒子的表面设置有镍-钨-硼导电层(厚度约0.1μm)的导电性粒子。
(参考例1)
将碳化钨粒子(平均粒径100nm)变更为镍粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(比较例1)
将碳化钨粒子(平均粒径100nm)变更为铜粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(比较例2)
将碳化钨粒子(平均粒径100nm)变更为二氧化硅粒子(平均粒径100nm)，除此以外，与实施例1同样地获得导电性粒子。
(实施例17)
(l)钯附着工序
准备粒径为3.0μm的二乙烯基苯树脂粒子(积水化学工业社制的“Micropearl SP-203”)。对该树脂粒子进行浸蚀，并进行水洗。接着，将树脂粒子添加至含有钯催化剂8重量％的钯催化剂液100mL中并进行搅拌。其后，进行过滤并进行清洗。将树脂粒子添加至pH值6的0.5重量％二甲基胺硼烷液中，获得附着有钯的树脂粒子。
(2)导电材料附着工序
在离子交换水400mL中对附着有钯的树脂粒子搅拌3分钟，使之分散而获得分散液。接着，历时3分钟将含有碳化钨粒子(平均粒径100nm)5重量％的浆料400g添加在获得的分散液中，从而获得了含有附着有导电材料的树脂粒子的悬浮液。
(3)非电解镀铜工序
准备含有硫酸铜0.23mol/L、乙二胺四乙酸盐2.3mol/L、福尔马林0.5mol/L的镀铜液(pH值12.5)。在60℃下对所获得的悬浮液进行搅拌，并且将上述镀铜液缓慢地滴加至悬浮液来进行非电解镀铜。其后，通过对悬浮液进行过滤而取出粒子，进行水洗并进行干燥，由此获得在树脂粒子的表面上配置有铜导电层(厚度0.1μm)的导电性粒子。
(评价)
(1)连接电阻
连接结构体的制作：
对双酚A型环氧树脂(三菱化学社制的“Epikote 1009”)10重量份、丙烯酸橡胶(重均分子量约80万)40重量份、甲基乙基酮200重量份、微胶囊型固化剂(旭化成chemicals社制的“HX3941HP”)50重量份、以及硅烷偶合剂(东丽道康宁硅社制的“SH6040”)2重量份进行混合，添加导电性粒子使得导电性粒子含量为3重量％，并使该导电性粒子分散来获得树脂组合物。
将所获得的树脂组合物涂布在单面经脱模处理的厚度50μm的PET(聚对苯二甲酸乙二醇酯)膜上，利用70℃的热风进行5分钟干燥，制作各向异性导电膜。所获得的各向异性导电膜的厚度为12μm。
将所获得的各向异性导电膜切割成5mm×5mm的尺寸。将切割得到的各向异性导电膜贴附在具有铝电极(高度0.2μm、L/S＝20μm/20μm)的玻璃基板(宽3cm、长3cm)的铝电极侧的大致中央，所述铝电极之一具有电阻测定用的线圈(引き回し線)。接着，使具有相同铝电极的2层挠性印制基板(宽2cm、长1cm)位置相配进行贴合从而使得电极彼此重叠。将该玻璃基板与2层挠性印制基板形成的叠层体在10N、180℃、以及20秒钟的压接条件下进行热压接，而获得连接结构体。需要说明的是，使用了铝电极直接形成在聚酰亚胺膜上的2层挠性印制基板。
连接电阻的测定：
利用四端子法对所获得的连接结构体的对置电极间的连接电阻进行测定。另外，利用下述基准判定连接电阻。
[连接电阻的评价基准]
○○：低于使用了参考例1中导电性粒子时的连接电阻的90％
○：使用了参考例1中导电性粒子时的连接电阻的90％以上且低于95％
△：使用了参考例1中导电性粒子时的连接电阻的95％以上且低于105％
×：使用了参考例1中导电性粒子时的情况的连接电阻的105％以上
将结果示于下述的表1、2。

Claims (12)

1.一种导电性粒子，其具有：基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的导电材料，
所述导电材料的材质为莫氏硬度高于镍的材质。
2.如权利要求1所述的导电性粒子，其具有：所述基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，
所述导电材料的材质为钼、碳化钨、钨、碳化钛或碳化钽。
3.如权利要求1或2所述的导电性粒子，其具有多个所述导电材料。
4.如权利要求1～3中任一项所述的导电性粒子，其具有：所述基体材料粒子、配置于所述基体材料粒子表面上的导电层、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，
所述导电材料被埋入所述导电层内。
5.如权利要求4所述的导电性粒子，其中，
所述导电层在外侧表面具有突起，且在所述导电层的所述突起的内侧配置有所述导电材料。
6.如权利要求4或5所述的导电性粒子，其中，
所述导电层具有镍层。
7.如权利要求4～6中任一项所述的导电性粒子，其中，
所述导电层在所述基体材料粒子侧具有镍层，在与所述基体材料粒子侧相反的一侧具有钯层。
8.如权利要求4～7中任一项所述的导电性粒子，其还具有附着于所述导电层表面的绝缘性物质。
9.如权利要求1～8中任一项所述的导电性粒子，其中，
所述导电材料为粒子。
10.如权利要求1～9中任一项所述的导电性粒子，其具有：所述基体材料粒子、以及配置于所述基体材料粒子表面上的部分区域的所述导电材料，
所述导电材料的材质为钼、碳化钨、钨或碳化钽。
11.一种导电材料，其含有权利要求1～10中任一项所述的导电性粒子和粘合剂树脂。
12.一种连接结构体，其具有：在表面具有第1电极的第1连接对象部件、在表面具有第2电极的第2连接对象部件、
将所述第1连接对象部件和所述第2连接对象部件连接的连接部，
所述连接部由权利要求1～10中任一项所述的导电性粒子形成，或由含有所述导电性粒子和粘合剂树脂的导电材料形成，
所述第1电极和所述第2电极通过所述导电性粒子实现了电连接。
CN201910187736.7A 2012-10-02 2013-09-30 导电性粒子、导电材料及连接结构体 Pending CN110000372A (zh)

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