CN105210157A - 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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CN105210157A
CN105210157A CN201480021985.4A CN201480021985A CN105210157A CN 105210157 A CN105210157 A CN 105210157A CN 201480021985 A CN201480021985 A CN 201480021985A CN 105210157 A CN105210157 A CN 105210157A
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mentioned
particle
electroconductive particle
jut
conductive part
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CN105210157B (zh
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山际仁志
笹平昌男
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Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01R—ELECTRICALLY-CONDUCTIVE CONNECTIONS; STRUCTURAL ASSOCIATIONS OF A PLURALITY OF MUTUALLY-INSULATED ELECTRICAL CONNECTING ELEMENTS; COUPLING DEVICES; CURRENT COLLECTORS
    • H01R13/00—Details of coupling devices of the kinds covered by groups H01R12/70 or H01R24/00 - H01R33/00
    • H01R13/02—Contact members
    • H01R13/03—Contact members characterised by the material, e.g. plating, or coating materials
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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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    • H01L24/83—Methods for connecting semiconductor or other solid state bodies using means for bonding being attached to, or being formed on, the surface to be connected using a layer connector
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    • H01R4/04—Electrically-conductive connections between two or more conductive members in direct contact, i.e. touching one another; Means for effecting or maintaining such contact; Electrically-conductive connections having two or more spaced connecting locations for conductors and using contact members penetrating insulation using electrically conductive adhesives
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    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
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Abstract

本发明提供一种导电性粒子，其对电极间进行电连接的情况下，可以降低连接电阻。本发明的导电性粒子1具备：基材粒子2、配置于基材粒子2表面上的导电部3，导电部3在外表面上具有多个突起3a，导电部3具有晶体结构，在导电部3的具有突起3a的部分和不具有突起3a的部分，晶体结构是连续的。

Description

导电性粒子、导电材料及连接结构体
技术领域
本发明涉及具备基材粒子和配置于该基材粒子表面上的导电部且上述导电部在外表面具有多个突起的导电性粒子。本发明还涉及使用了上述导电性粒子的导电材料及连接结构体。
背景技术
各向异性导电糊剂及各向异性导电膜等各向异性导电材料已广为人知。对上述各向异性导电材料而言，在粘合剂树脂中分散有导电性粒子。
为了得到各种连接结构体，上述各向异性导电材料可用于例如挠性印刷基板和玻璃基板的连接(FOG(FilmonGlass))、半导体芯片和挠性印刷基板的连接(COF(ChiponFilm))、半导体芯片和玻璃基板的连接(COG(ChiponGlass))以及挠性印刷基板和玻璃环氧基板的连接(FOB(FilmonBoard))等。另外，作为上述导电性粒子，有时使用具有基材粒子和配置于该基材粒子表面上的导电部的导电性粒子。
作为上述导电性粒子的一个例子，下述专利文献1中公开了芯材粒子(基材粒子)和在该芯材粒子的表面具有金属或合金覆膜的导电性粒子。该导电性粒子具有从上述包膜的表面突出的多个突起部。上述突起部由将金属或合金的多个粒子连结成列状而形成的粒子连结体构成。专利文献1的实施例及比较例中公开有连结突起部的比例为32％以上的导电性粒子。
下述专利文献2中公开有一种通过非电解镀敷法在平均粒径1～20μm的球状的基材粒子表面上形成有镍导电层或镍合金导电层的导电性粒子。该导电性粒子在导电层的最表层具有0.05～4μm的微小突起。该导电层和该突起实际上连续地排列。作为上述基材粒子，可使用树脂粒子。
现有技术文献
专利文献
专利文献1：日本特开2012-113850号公报
专利文献2：日本特开2000-243132号公报
发明内容
发明所要解决的问题
近年来，要求降低电子设备的耗电量。因此，对导电性粒子要求可以进一步降低由导电性粒子进行电连接的电极间连接电阻的性质。
但是，如使用专利文献1、2所记载的现有导电性粒子对电极间进行电连接的情况下，有时连接电阻变高。
大多情况下，在电极表面及导电性粒子的表面形成有氧化膜。专利文献1、2所记载的导电性粒子中，在进行电极间的连接时，突起容易折断，作为结果，有时突起不能充分贯穿氧化膜。因此，有时电极间的连接电阻变高。
本发明的目的在于，提供一种导电性粒子，在对电极间进行电连接的情况下，可以降低连接电阻。本发明的另一目的在于，提供一种使用了所述导电性粒子的导电材料及连接结构体。
解决问题的技术方案
根据本发明的宽泛方面，提供一种导电性粒子，其具备：基材粒子以及配置于所述基材粒子表面上的导电部，所述导电部在外表面具有多个突起，
所述导电部具有晶体结构，在所述导电部的具有所述突起的部分和不具有所述突起的部分，晶体结构是连续的。
在本发明的导电性粒子的某个特定方面，所述导电部由金属或金属合金形成，所述突起具有多个第一突起部，所述第一突起部由所述金属或金属合金形成，而不是由多个所述金属或金属合金的粒子连结成列状而形成，所述突起不具有由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部，或者具有至少一个由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部，所述第一突起部和所述第二突起部的总个数100％中的70％以上为所述第一突起部。
在本发明的导电性粒子的某个特定方面，所述第一突起部和所述第二突起部的总个数100％中的90％以上为所述第一突起部。
在本发明的导电性粒子的某个特定方面，所述导电部中的微晶尺寸为0.1nm以上、100nm以下。
在本发明的导电性粒子的某个特定方面，所述导电部的晶格应变为0.001％以上、且10％以下。
在本发明的导电性粒子的某个特定方面，所述导电部含有镍。
在本发明的导电性粒子的某个特定方面，所述导电性粒子在所述导电部的内部及内侧不具有用于使所述导电部的外表面隆起的芯物质。
在本发明的导电性粒子的某个特定方面，所述突起的高度为所述导电性粒子的粒径的1/100以上。
在本发明的导电性粒子的某个特定方面，所述导电性粒子具备配置于所述导电部外表面上的绝缘性物质。
根据本发明的宽泛方面，提供一种连接结构体，其具备：第一连接对象部件，其表面具有第一电极；第二连接对象部件，其表面具有第二电极；连接部，其将所述第一连接对象部件和所述第二连接对象部件连接在一起，所述连接部由所述导电性粒子形成，或者由含有所述导电性粒子和粘合剂树脂的导电材料形成，所述第一电极和所述第二电极通过所述导电性粒子实现了电连接。
发明的效果
本发明的导电性粒子具备基材粒子和配置于所述基材粒子表面上的导电部，所述导电部在外表面具有多个突起，所述导电部具有晶体结构，在所述导电部的具有所述突起的部分和不具有所述突起的部分，晶体结构是连续的，因此，在使用本发明的导电性粒子对电极间进行电连接的情况下，可以降低连接电阻。
附图说明
图1是表示本发明第一实施方式的导电性粒子的剖面图；
图2是表示本发明第二实施方式的导电性粒子的剖面图；
图3是表示本发明第三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了本发明第一实施方式的导电性粒子的连接结构体的剖面图。
标记说明
1，1A，1B…导电性粒子
1a，1Aa，1Ba…突起
2，2A…基材粒子
2Ax…有机核
2Ay…无机壳
3，3A，3B…导电部
3a，3Aa…突起
3Bx…第一导电部
3By…第二导电部
3Bya…突起
4…芯物质
5…绝缘性物质
51…连接结构体
52…第一连接对象部件
52a…第一电极
53…第二连接对象部件
53a…第二电极
54…连接部
54a…粘合剂树脂
具体实施方式
以下，说明本发明的详细情况。
(导电性粒子)
本发明的导电性粒子具备基材粒子和配置于上述基材粒子表面上的导电部。本发明的导电性粒子中，上述导电部在外表面具有多个突起。本发明的导电性粒子中，上述导电部具有晶体结构。本发明的导电性粒子中，在所述导电部的具有所述突起的部分和不具有所述突起的部分，晶体结构是连续的。
通过采用本发明的导电性粒子中的上述构成，在使用本发明的导电性粒子对电极间进行电连接的情况下，可以降低连接电阻。作为其原因，认为由于晶体结构是连续的，变得硬质且延展性变高，结果突起变得比较硬。
本发明中，从降低电极间的连接电阻的观点出发，在所述导电部的具有所述突起的部分和不具有所述突起的部分，晶体结构是连续的。不具有上述突起的部分为导电部的第一部分，具有突起的部分是厚度比第一部分厚的第二部分。第一部分中，导电部的外表面不隆起。
从有效地降低电极间的连接电阻的观点出发，上述导电部的微晶尺寸优选为0.1nm以上，更优选为1.73nm以上，进一步优选为5nm以上，优选为100nm以下，更优选为50nm以下，进一步优选为10nm以下。作为其原因，若上述导电部的微晶尺寸为上述下限以上及上述上限以下，则更进一步变得硬质，且延展性更进一步变高，结果突起变得比较硬。在满足上述微晶尺寸的导电部中，在进行电极间的连接时，突起不易折断，且突起不易损伤。本发明中，通过形成满足上述微晶尺寸的导电部，突起充分贯穿电极或导电性粒子表面的氧化膜，因此，可以更进一步降低电极间的连接电阻。
从有效地降低电极间的连接电阻的观点出发，上述导电部的晶格应变优选为0.001％以上，更优选为0.01％以上，进一步优选为0.1％以上，特别优选为0.15％以上，优选为10％以下，更优选为5％以下，进一步优选为1％以下。
为了使上述微晶尺寸、上述晶体结构的连续性及上述晶格应变在本发明的导电性粒子中最优选化，适当进行使发生共析的金属相对于主金属的比例的最优选化，镀敷反应速度的最优选化、镀浴中pH的最优选化及镀浴中温度的最优选化等。
作为使上述导电部的微晶尺寸微细化的方法，可举出：镍导电部中磷含量的增加引起的微细化、镍导电部中的硼含量的增加引起的微细化、镀液中的有机类光泽剂的添加引起的微细化以及金属类光泽剂的添加引起的微细化的方法等。特别是镀镍导电部中的磷及硼含量的增加、有机类光泽剂的添加对导电部的微晶尺寸的微细化具有效果。
作为增加镀镍导电部中磷及硼含量的方法，可举出：降低镀液的pH来延缓镀镍液的反应速度的方法、降低镀镍液温度的方法、提高镀镍液中磷类还原剂及硼类还原剂的浓度的方法、提高镀镍液中络化剂的浓度的方法等。这些方法也可以单独使用一种，也可以组合使用两种以上。
作为上述有机类光泽剂，可举出：糖精、萘二磺酸钠、萘三磺酸钠、烯丙基磺酸钠、炔丙基磺酸钠、丁炔二醇、炔丙醇、香豆素、福尔马林、乙氧基化聚乙烯亚胺、多烷基亚胺、聚乙烯亚胺、明胶、糊精、硫脲、聚乙烯醇、聚乙二醇、聚丙烯酰胺、肉桂酸、烟酸及亚苄基丙酮等。上述有机类光泽剂可以单独使用一种，也可以组合使用两种以上。
另外，作为上述有机类光泽剂优选的例子，可举出：乙氧基化聚乙烯亚胺、多烷基亚胺、聚乙烯亚胺及聚乙二醇等。
作为降低上述导电部中的晶格应变的方法，可举出向镀液中添加金属稳定剂的方法等。通过上述金属稳定剂的添加，镀液的稳定性提高，晶格应变减少，可形成对基材粒子的包覆性良好的镀膜。作为上述金属稳定剂，可举出：铅化合物、铋化合物、铊化合物及钒化合物等。作为上述金属稳定剂的具体例，可举出：构成化合物的金属(铅、铋、铊、钒)的硫酸盐、碳酸盐、酢酸盐、硝酸盐及盐酸盐等。当考虑对环境的影响时，优选为：铋化合物、铊化合物或钒化合物。
上述导电性粒子的上述突起的高度优选为0.001μm以上，更优选为0.05μm以上，优选为0.9μm以下，更优选为0.2μm以下。若上述突起的高度为上述下限以上及上述上限以下，则电极间的连接电阻有效地降低。上述突起的高度是每个导电性粒子的多个突起高度的平均。上述突起的高度表示：连接导电性粒子的中心和突起顶端的线(图1所示的虚线L1)上的、从假定无突起时的导电部的假想线(图1所示的虚线L2)上起(假定无突起时的球状的导电性粒子的外表面上)到突起顶端的距离。即，表示图1中从虚线L1和虚线L2的交点到突起顶端的距离。
从有效地降低连接电阻且有效地提高电极间的连接可靠性的观点出发，优选上述突起的高度为上述导电性粒子的粒径的1/100以上，更优选为1/15以上。另外，突起高度优选为导电性粒子的粒径的1/6以下。此外，在后述的实施例中，突起高度全部为导电性粒子的粒径的1/15以上、1/6以下。
上述每个导电性粒子的上述突起优选为3个以上，更优选为5个以上。上述突起数的上限不具有特别限定。突起数的上限可考虑导电性粒子的粒径等适当选择。上述导电部外表面的整个表面面积100％中，具有上述突起的部分的表面面积优选为30％以上，更优选为50％以上。
上述突起可以具有多个第一突起部，所述第一突由所述金属或金属合金形成，而不是由多个所述金属或金属合金的粒子连结成列状而形成。上述突起可以不具有由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部，或者具有至少一个由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部。本发明的导电性粒子中，上述第一突起部和上述第二突起部的总个数100％中的70％以上优选为上述第一突起部。在该情况下，电极间的连接电阻更进一步降低。但是，上述第一突起部和上述第二突起部的总个数100％中的不足70％也可以是上述第一突起部，在该情况下，如果在上述导电部的具有上述突起的部分和不具有上述突起的部分，晶体结构是连续的，则也可得到本发明的效果。
上述第二突起部与上述第一突起部相比，在进行电极间的连接时，容易折断或损伤。因此，当上述第一突起部所占上述第一突起部和上述第二突起部的总个数的比例变少(例如不足70％)，且上述第二突起部的比例变多时(例如30％以上)，突起不能充分贯穿电极或导电性粒子表面的氧化膜，从而存在电极间的连接电阻容易变高的倾向。与此相对，通过上述第一突起部所占上述第一突起部和上述第二突起部的总个数的比例较多，突起充分贯穿电极或导电性粒子表面的氧化膜，因此，可以更进一步降低电极间的连接电阻。
已知有在导电部外表面具有多个突起的导电性粒子。另外，日本特开2012-113850号公报中，公开了导电性粒子，其具有由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体构成的突起。日本特开2012-113850号公报的实施例及比较例中，公开有连结突起部的比例为32％以上的导电性粒子。但是，在具有如上所述连结突起部的导电性粒子中，若连结突起部的比例较大，则电极间的连接电阻有时不能充分降低。与此相对，本发明的导电性粒子中，无连结突起部或连结突起部的比例较少，因此，可以充分降低电极间的连接电阻。
所述第一突起部由所述金属或金属合金形成，而不是由多个所述金属或金属合金的粒子连结成列状而形成。上述第一突起部是除上述粒子连结体以外的突起部。上述第二突起部由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成。上述突起通过上述第一突起和上述第二突起这两种突起形成。构成上述第二突起部及上述粒子连结体的各个粒子由形成导电部的金属或金属合金形成。另外，上述第一突起及上述第二突起可以是在直线状部分混有分支出的突起部而形成的形状。关于分支的个数及分支形式，可以分支为两个分支或多个分支，也可以是树枝状。
从更进一步降低电极间的连接电阻的观点出发，上述第一突起部和上述第二突起部的总个数100％中的上述第一突起部的个数比例更优选为80％以上，进一步优选为90％以上，特别优选为95％以上，上述第二突起部的个数比例更优选为不足30％，进一步优选为不足20％，特别优选为不足10％，最优选为不足5％。
上述第一突起部和上述第二突起部的总个数100％中的上述第二突起部的比例可以是1％以上，上述第一突起部的比例可以是99％以下。
上述第一突起部和上述第二突起部如下计数。
利用扫描电子显微镜(SEM)将倍率设定成25000倍，随机选择10个粒子，观察各个粒子的突起部。对于全部突起部分类成下列突起部：由所述金属或金属合金形成，而不是由多个所述金属或金属合金的粒子连结成列状而形成的突起部；和由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体形成的突起部。金属或金属合金的粒子是否多个连结可以通过在上述金属或金属合金的粒子间是否观察到晶界而判断。
从有效地降低电极间的连接电阻的观点出发，上述第一突起部的高度优选为上述导电部的不具有上述突起的部分的厚度的0.5倍以上，更优选为2倍以上，进一步优选为3倍以上，且优选为10倍以下，更优选为7倍以下。上述第一突起部的高度是每个导电性粒子的第一突起部高度的平均值。
上述第一突起部的高度表示连接导电性粒子的中心和第一突起部顶端的线(图1所示的虚线L1)上的、从假定不具有第一突起部时导电部的假想线(图1所示的虚线L2)上起(假定不具有第一突起部时球状的导电性粒子的外表面上)到第一突起部顶端的距离。即，表示图1中从虚线L1和虚线L2的交点到第一突起部的顶端的距离。另外，在第一突起部为分支得到的突起部的情况下，第一突起部的顶端是最远离导电性粒子外表面的突起部的顶端部分。
从有效地降低电极间的连接电阻的观点出发，上述第一突起部的宽度优选为上述导电部的不具有上述突起的部分的厚度的0.1倍以上，更优选为0.5倍以上，进一步优选为1倍以上，且优选为5倍以下，更优选为3倍以下。上述第一突起部的宽度是与上述第一突起部的高度方向垂直方向上的最大直径。
从有效地降低电极间的连接电阻的观点出发，上述第二突起部的高度优选为上述导电部的不具有上述突起的部分的厚度的0.5倍以上，更优选为2倍以上，进一步优选为3倍以上，且优选为10倍以下，更优选为7倍以下。上述第二突起部的高度是每个导电性粒子的第二突起部高度的平均值。
上述第二突起部的高度与上述第一突起部的高度一样地定义。即，上述第二突起部的高度表示：连接导电性粒子的中心和第二突起部顶端的线上的、从假定不具有第二突起部时导电部的假想线上起(假定不具有第二突起部时球状导电性粒子的外表面上)到第二突起部顶端的距离。在第二突起部为分支得到的突起部的情况下，第二突起部的顶端是最远离导电性粒子的外表面的突起部的顶端部分。
从有效地降低电极间的连接电阻的观点出发，上述第二突起部的宽度优选为上述导电部的不具有上述突起的部分的厚度的0.1倍以上，更优选为0.5倍以上，进一步优选为1倍以上，且优选为5倍以下，更优选为3倍以下。上述第二突起部的宽度是与上述第二突起部的高度方向垂直方向上的最大直径。
构成上述第二突起部的上述金属或金属合金的粒子的粒径优选为10nm以上，更优选为20nm以上，优选为500nm以下，更优选为400nm以下。构成上述第二突起部的上述金属或金属合金的粒子的粒径为上述下限以上及上述上限以下时，电极间的连接电阻更进一步降低。构成上述第二突起部的上述金属或金属合金的粒子的粒径是指最大直径。
上述第一突起部具体而言为不是由多个所述金属或金属合金的粒子连结成列状而形成的突起部，利用扫描电子显微镜(SEM)观察时，是与在金属或金属合金的粒子间确认到晶界的突起部不同的突起部。
上述第二突起部中，在利用扫描电子显微镜(SEM)观察时，在上述金属或金属合金的粒子间观察到晶界。根据该事实确认到：上述第二突起部通过多个上述金属或金属合金的粒子连结而形成。就上述第一突起部而言，在上述金属或金属的合金中未观察到晶界。
上述第一突起部和上述第二突起部利用扫描电子显微镜(SEM)进行识别。上述第一突起部中不存在晶界，因此，不是粒子连结体。
多个上述金属或金属合金的粒子通过连结成列状，形成上述第二突起部。关于连结成列状，多个上述金属或金属合金的粒子是指发生了连接，使其向某个方向延伸。上述第二突起部也可以例如将多个上述金属或金属合金的粒子连结成直线状而构成，也可以通过对多个上述金属或金属合金的粒子进行连结，形成蛇行形状的第二突起部。另外，直线状部和蛇行部也可以混合存在。另外，上述第二突起部可以在从导电部侧的基部到朝向顶端部之间进行多个分支。例如上述第二突起部可以是Y字状等。着眼于一个导电性粒子时，存在的多个第二突起部的形状可以相同，也可以不同。
多个第二突起部中，上述金属或金属合金的粒子数可以相同，也可以不同。上述第二突起部通过将至少两个上述金属或金属合金的粒子连结成列状而构成。上述第二突起部的上述金属或金属合金的粒子的连结个数为2以上，优选为30以下，更优选为20以下，进一步优选为5以下，特别优选为3以下。构成上述第二突起部的上述金属或金属合金的粒子数通过利用扫描电子显微镜(SEM)观察上述第二突起部进行测量。
从使电极间的连接电阻更进一步良好的观点出发，每一个导电性粒子的上述第一突起部和上述第二突起部的总个数优选为5个以上，更优选为10个以上，进一步优选为20个以上，优选为1000个以下，更优选为500个以下，进一步优选为300个以下。
作为相比于上述第二突起部更易于形成上述第一突起部的方法，可举出使用高分子量的络化剂的方法以及使用硫黄类稳定剂的方法等。通过使用高分子量的络化剂，络合物的尺寸变大，络合物不易进入多个突起间，可以仅使突起部选择性地成长。
将上述导电性粒子压缩10％时的压缩弹性模量(10％K值)优选为1000N/mm2以上，更优选为5000N/mm2以上，进一步优选为6300N/mm2以上，优选为20000N/mm2以下，更优选为16000N/mm2以下。当上述10％K值为上述下限以上及上述上限以下时，电极间的连接电阻有效地降低。
上述导电性粒子的上述压缩弹性模量(10％K值)可如下测定。
使用微小压缩试验机，利用圆柱(直径100μm，金刚石制)的平滑压头端面，在25℃、压缩速度0.3mN/秒及最大试验负荷20mN的条件下压缩导电性粒子。测定此时的载荷值(N)及压缩位移(mm)。根据得到的测定值，可以通过下式求得上述压缩弹性模量。作为上述微小压缩试验机，例如，可使用Fischer株式会社制造“FischerscopeH-100”等。
10％K值(N/mm2)＝(3/21/2)·F·S-3/2·R-1/2
F：导电性粒子压缩变形10％时的载荷值(N)
S：导电性粒子压缩变形10％时的压缩位移(mm)
R：导电性粒子的半径(mm)
上述压缩弹性模量普遍且定量地表示导电性粒子的硬度。通过使用上述压缩弹性模量，可以定量且唯一地表示导电性粒子的硬度。
上述导电性粒子的粒径优选为0.5μm以上，更优选为1μm以上，优选为500μm以下，更优选为100μm以下，进一步优选为50μm以下，特别优选为20μm以下，最优选为10μm以下。若导电性粒子的粒径为上述下限以上及上述上限以下，则在使用导电性粒子对电极间实现连接的情况下，导电性粒子和电极的接触面积充分变大，且在形成导电部时不易形成凝聚的导电性粒子。另外，经由导电性粒子连接的电极间的间隔不会过大，且导电部不易从基材粒子表面剥离。
上述导电性粒子的粒径表示数均粒径。导电性粒子的数均粒径通过利用电子显微镜或光学显微镜观察50个任意的导电性粒子，并算出平均值而求得。
以下，通过参照附图说明本发明具体的实施方式及实施例，使本发明变得明确。此外，参照的附图中，为了便于图示，大小及厚度等从实际的大小及厚度进行适当变更。此外，各实施方式中的不同的部分结构可以适当置换、组合。
图1是表示本发明第一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具有基材粒子2和配置于基材粒子2的表面上的导电部3。导电性粒子1中，导电部3为导电层。导电部3包覆基材粒子2的表面。导电性粒子1是基材粒子2的表面被导电部3包覆而形成的包覆粒子。
导电性粒子1在导电性表面上具有多个突起1a。导电部3在外表面上具有多个突起3a。
导电部3具有第一部分和厚度比该第一部分厚的第二部分。因此，导电部3在表面(导电层的外表面)上具有突起3a。除多个突起1a和突起3a之外的部分是导电部3的上述第一部分。多个突起1a和突起3a是导电部3的厚度较厚的上述第二部分。
图2是表示本发明第二实施方式的导电性粒子的剖面图。
图2所示的导电性粒子1A具有基材粒子2和配置于基材粒子2的表面上的导电部3A。导电部3A为导电层。导电性粒子1和导电性粒子1A中，仅是否具有芯物质4不同。导电性粒子1A具有芯物质。
导电性粒子1A在基材粒子2的表面上具有多个芯物质4。导电部3A包覆基材粒子2和芯物质4。通过导电部3A包覆芯物质4，导电性粒子1A在表面上具有多个突起1Aa，导电部3A在外表面上具有多个突起3Aa。导电部3A的表面利用芯物质4而隆起，形成有多个突起1Aa。
如导电性粒子1A，为了形成突起1Aa和突起3Aa，可以使用芯物质，但优选不使用芯物质。
图3是表示本发明第三实施方式的导电性粒子的剖面图。
图3所示的导电性粒子1B具有：基材粒子2A、配置于基材粒子2A表面上的导电部3B和绝缘性物质5。导电部3B为导电层。导电部3B具有配置于基材粒子2A表面上的第一导电部3Bx和配置于第一导电部3Bx表面上的第二导电部3By。
基材粒子2A为有机无机杂化粒子。基材粒子2A具有有机核2Ax和配置于有机核2Ax表面上的无机壳2Ay。
导电性粒子1B在导电性的表面上具有突起1Ba。导电性粒子1B在表面上具有突起1Ba。导电部3B在表面(导电层的外表面)上具有突起3Ba。第二导电部3By具有第一部分和厚度比该第一部分厚的第二部分。因此，第二导电部3By在表面(导电层的外表面)上具有突起3Bya。除多个突起3Bya之外的部分是第二导电部3By的上述第一部分。多个突起3Bya是第二导电部3By的厚度较厚的上述第二部分。
如导电性粒子1B，导电部3B也可以具有多层结构。另外，为了形成突起1Ba和突起3Ba，也可以将芯物质4配置于内层的第一导电部3Bx上，并利用外层的第二导电部3By包覆芯物质4及第一导电部3Bx。
导电性粒子1B具备导电部3B及配置于第二导电部3By外表面上的绝缘性物质5。导电部3B及第二导电部3By外表面的至少一部分区域被绝缘性物质5包覆。绝缘性物质5利用具有绝缘性的材料形成，是绝缘性粒子。如上所述，本发明的导电性粒子可以具有配置于导电部外表面上的绝缘性物质。
上述导电性粒子1、导电性粒子1A和导电性粒子1B中，导电部3、导电部3A和导电部3By具有晶体结构，在导电部3、导电部3A和导电部3By的具有突起3a、突起3Aa和突起3Bya的部分和不具有突起3a、突起3Aa和突起3Bya的部分，晶体结构是连续的。上述的导电性粒子1、导电性粒子1A和导电性粒子1B中，导电部3、导电部3A和导电部3By的微晶尺寸优选为0.1nm以上，优选为100nm以下。
以下，说明导电性粒子的其它详情。
[基材粒子]
作为上述基材粒子，可举出：树脂粒子、除金属粒子之外的无机粒子、有机无机杂化粒子及金属粒子等。上述基材粒子优选为除金属粒子之外的基材粒子，更优选为树脂粒子、除金属粒子之外的无机粒子或有机无机杂化粒子。上述基材粒子可以是核壳粒子。
上述基材粒子进一步优选为树脂粒子或有机无机杂化粒子，可以是树脂粒子，也可以是有机无机杂化粒子。通过使用这些优选的基材粒子，且通过对电极间进行电连接，可得到更优选的导电性粒子。
在使用上述导电性粒子对电极间进行连接时，在将上述导电性粒子配置于电极间后，通过压接而压缩上述导电性粒子。若基材粒子为树脂粒子或有机无机杂化粒子，则在进行上述压接时，上述导电性粒子易于变形，导电性粒子和电极的接触面积变大。因此，电极间的连接电阻更进一步降低。
作为用于形成上述树脂粒子的树脂，优选使用各种有机物。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、聚偏二氯乙烯、聚异丁烯、聚丁二烯等聚烯烃树脂；聚甲基丙烯酸甲酯、聚丙烯酸甲酯等丙烯酸树脂；聚对苯二甲酸亚烷基酯、聚碳酸酯、聚酰胺、苯酚甲醛树脂、三聚氰胺甲醛树脂、苯并胍胺甲醛树脂、脲甲醛树脂、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、聚砜、聚苯醚、聚缩醛、聚酰亚胺、聚酰胺酰亚胺、聚醚醚酮、聚醚砜及由一种或两种以上的具有烯属不饱和基团的各种聚合性单体经聚合而得到的聚合物。可以设计及合成具有进行任意压缩时适于导电性材料物性的树脂粒子，且可容易将基材粒子的硬度控制在优选的范围，因此，用于形成上述树脂粒子的树脂优选为使一种或两种以上的具有多个烯属不饱和基团的聚合性单体进行聚合而成的聚合物。
在使具有烯属不饱和基团的单体进行聚合而得到上述树脂粒子的情况下，作为上述具有烯属不饱和基团的单体，可举出非交联性的单体和交联性的单体。
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类单体；(甲基)丙烯酸、马来酸、马来酸酐等含羧基的单体；(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)丙烯酸鲸蜡酯、(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-羟乙酯、(甲基)丙烯酸甘油酯、(甲基)丙烯酸聚氧乙烯酯、(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)丙烯腈等含腈的单体；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、氯苯乙烯等含卤素的单体等。
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-丁烷二醇二醇二(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、邻苯二甲酸二烯丙酯、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。
通过利用公知的方法使上述具有烯属不饱和基团的聚合性单体聚合，可以得到上述树脂粒子。作为其方法，例如可举出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并聚合的方法等。
上述基材粒子为除金属粒子之外的无机粒子或有机无机杂化粒子的情况下，作为用于形成上述基材粒子的无机物，可举出二氧化硅、氧化铝、钛酸钡、氧化锆及碳黑等。上述无机物优选不是金属。作为由上述二氧化硅形成的粒子，没有特别限定，例如，可举出如下得到的粒子：通过对具有2个以上的水解性烷氧基甲硅烷基的硅化合物进行水解而形成交联聚合物粒子，然后，根据需要进行烧成。作为上述有机无机杂化粒子，例如，可举出由交联后的烷氧基甲硅烷聚合物和丙烯酸树脂形成的有机无机杂化粒子等。
上述有机无机杂化粒子优选为具有核和配置于该核表面上的壳的核壳型有机无机杂化粒子。上述核优选为有机核。上述壳优选为无机壳。从有效地降低电极间的连接电阻的观点出发，上述基材粒子优选为具有有机核和配置于上述有机核表面上的无机壳的有机无机杂化粒子。
作为用于形成上述有机核的材料，可举出用于形成上述树脂粒子的树脂等。
作为用于形成上述无机壳的材料，可举出用于形成上述基材粒子的无机物。用于形成上述无机壳的材料优选为二氧化硅。上述无机壳优选如下形成：在上述核表面上，将金属烷氧化物通过溶胶凝胶法形成壳状物后，烧成该壳状物。上述金属烷氧化物优选为硅烷氧化物。上述无机壳优选由硅烷氧化物形成。
在上述基材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。但是，上述基材粒子优选不是金属粒子。
上述基材粒子的粒径优选为0.1μm以上，更优选为0.5μm以上，进一步优选为2μm以上，优选为30μm以下，更优选为10μm以下。上述基材粒子的粒径也可以是5μm以下，也可以是3μm以下。若上述基材粒子的粒径为上述下限以上及上述上限以下，则电极间的间隔变小，且即使增厚导电部的厚度，也可得到较小的导电性粒子。
上述基材粒子的粒径在基材粒子为真球状的情况下表示直径，在基材粒子不是真球状的情况下表示最大直径。
[导电部]
上述导电部的不具有上述突起的部分的厚度优选为0.005μm以上，更优选为0.01μm以上，优选为1μm以下，更优选为0.3μm以下。上述导电部的不具有上述突起的部分的厚度为上述下限以上及上述上限以下时，可得到充分的导电性，且导电性粒子不会过硬，在连接电极间时，导电性粒子充分变形。
在由多层形成上述导电部的情况下，最外层的导电层的不具有上述突起的部分的厚度特别是最外层为金层时，金层的厚度优选为0.001μm以上，更优选为0.01μm以上，优选为0.5μm以下，更优选为0.1μm以下。上述最外层的导电层的不具有上述突起的部分的厚度为上述下限以上及上述上限以下时，最外层的导电层进行的包覆均匀，抗腐蚀性充分提高，且电极间的连接电阻充分降低。
上述导电部的不具有上述突起部分的厚度可以通过使用例如透射电子显微镜(TEM)观察导电性粒子的截面进行测定。
作为在上述基材粒子的表面上形成上述导电部的方法，可举出通过非电解镀敷形成上述导电部的方法以及通过电镀形成上述导电部的方法等。
上述导电部优选含有金属。作为上述导电部材料的金属没有特别限定。作为该金属，例如可举出：金、银、铜、铂、钯、锌、铅、铝、钴、铟、镍、铬、钛、锑、铋、锗及镉以及它们的合金等。另外，作为上述金属，也可以使用锡掺杂氧化铟(ITO)。这些金属可以在导电部内合金化。但是，为了将上述导电部的结晶化度设为上述下限以上及上述上限以下，可选择适当的金属。上述金属可以单独使用一种，也可以组合使用两种以上。
从有效地降低电极间的连接电阻且将上述导电部的结晶化度控制在更进一步优选的范围的观点出发，上述导电部优选含有铜或镍，且优选含有镍。在该情况下，镍等金属也可以与其它金属合金化。上述导电部的材料优选为铜、铜合金、镍或镍合金，更优选为镍或镍合金。
在外表面上具有多个突起的上述导电部100重量％中，铜或镍的含量优选为10重量％以上，更优选为25重量％以上，进一步优选为40重量％以上，优选为100重量％(全量)以下。上述导电部中的镍含量优选为上述下限以上及上述上限以下。
上述导电部优选含有作为主金属的镍。含有镍的导电部整体100重量％中，镍含量优选为50重量％以上。含有镍的导电部100重量％中，镍含量优选为65重量％以上，更优选为80重量％以上，进一步优选为90重量％以上。当镍含量为上述下限以上时，电极间的连接电阻进一步降低。
从更进一步降低电极间的连接电阻的观点出发，含有镍的导电部优选含有磷或硼，更优选含有磷。含有镍的导电部整体100重量％中，磷含量优选为超过0重量％，更优选为0.1重量％以上，进一步优选为2重量％以上，特别优选为5重量％以上，最优选超过10重量％，优选为20重量％以下，更优选为15重量％以下。若含磷量为上述下限以上及上述上限以下，则连接电阻更进一步降低。特别是若磷含量为5重量％以上，则连接电阻的可靠性更进一步提高，若磷含量超过10重量％，则密合性提高，且连接电阻的可靠性更进一步提高。
作为控制上述导电部中的镍、硼及磷的含量的方法，例如可举出：在通过非电解镀镍形成导电部时控制镍镀液的pH的方法、通过非电解镀镍形成导电部时调整含硼还原剂的浓度的方法、通过非电解镀镍形成导电部时调整含磷还原剂的浓度的方法以及调整镍镀液中的镍浓度的方法等。
在通过非电解镀敷形成的方法中，一般进行催化剂化工序和非电解镀敷工序。以下，对通过非电解镀敷在树脂粒子的表面上形成含有镍和磷的合金镀层的方法的一个例子进行说明。
上述催化剂化工序中，使用于通过非电解镀敷形成镀敷层的起点即催化剂在树脂粒子的表面形成。
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，通过酸溶液或碱溶液使树脂粒子的表面活性化，并在树脂粒子的表面上析出钯的方法；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使树脂粒子的表面活性化，并在树脂粒子的表面上析出钯的方法等。作为上述还原剂，优选使用含磷还原剂。另外，作为上述还原剂，通过使用含硼还原剂，可形成含有硼的导电层。
上述非电解镀敷工序中，优选使用含有含镍化合物及上述含磷还原剂的镍镀浴。通过在镍镀浴中浸渍树脂粒子，可以在表面形成有催化剂的树脂粒子的表面上析出镍，可以形成含有镍和磷的导电层。
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。
作为上述含磷还原剂，可举出次亚磷酸钠等。作为上述含硼还原剂，可举出二甲胺硼烷、硼氢化钠及硼氢化钾等。
[芯物质]
通过将上述芯物质埋入上述导电部中，容易使上述导电部在外表面上具有多个突起。但是，为了在导电性粒子及导电部的表面上形成突起，未必一定使用芯物质，优选不使用芯物质。上述导电性粒子优选在上述导电部的内部及内侧不具有用于使上述导电部的外表面隆起的芯物质。上述导电部优选在上述导电部的内部及内侧不含有用于使上述导电部的外表面隆起的芯物质。优选在球状的基材粒子表面上形成外表面具有突起的导电部而不使用芯物质。
作为在上述导电性粒子的表面上形成突起的方法，可举出：在基材粒子的表面上附着芯物质后，通过非电解镀敷形成导电部的方法；以及在基材粒子的表面上通过非电解镀敷形成导电部后，附着芯物质，并进一步通过非电解镀敷形成导电部的方法等。作为形成上述突起的其它方法，可举出：在基材粒子的表面上形成第一导电部后，在该第一导电部上配置芯物质，然后形成第二导电部的方法；以及在基材粒子的表面上形成导电部的中途阶段添加芯物质的方法等。
作为在上述基材粒子的表面上配置芯物质的方法，例如可举出：向基材粒子的分散液中添加芯物质，且使芯物质通过例如范德瓦尔斯力集聚、附着于基材粒子的表面的方法；以及向加入有基材粒子的容器中添加芯物质，通过容器旋转等产生的机械作用使芯物质附着于基材粒子的表面的方法等。其中，为了易于控制附着的芯物质的量，优选使芯物质集聚、附着于分散液中的基材粒子表面上方法。
作为上述芯物质的材料，可举出导电性物质及非导电性物质。作为上述导电性物质，例如可举出：金属、金属氧化物、石墨等导电性非金属及导电性聚合物等。作为上述导电性聚合物，可举出聚乙炔等。作为上述非导电性物质，可举出二氧化硅、氧化铝及氧化锆等。其中，为了提高氧化膜的贯穿效果，优选芯物质较硬。上述芯物质优选为金属粒子。作为上述芯物质的材料的金属，可以适当使用作为上述导电材料的材料所例举的金属。
作为上述芯物质的材料的具体例，可举出：钛酸钡(莫氏硬度4.5)、镍(莫氏硬度5)、二氧化硅(二氧化硅、莫氏硬度6～7)、氧化钛(莫氏硬度7)、氧化锆(莫氏硬度8～9)、氧化铝(莫氏硬度9)、碳化钨(莫氏硬度9)及金刚石(莫氏硬度10)等。上述无机粒子优选为：镍、二氧化硅、氧化钛、氧化锆、氧化铝、碳化钨或金刚石，更优选为：二氧化硅、氧化钛、氧化锆、氧化铝、碳化钨或金刚石，进一步优选为：氧化钛、氧化锆、氧化铝、碳化钨或金刚石，特别优选为：氧化锆、氧化铝、碳化钨或金刚石。上述芯物质的材料的莫氏硬度优选为5以上，更优选为6以上，进一步优选为7以上，特别优选为7.5以上。
上述芯物质的形状没有特别限。芯物质的形状优选为块状。作为芯物质，例如可举出：粒子状块、多个微小粒子凝聚而成的凝聚块及无定形块等。
作为上述金属，例如可举出由下列两种以上的金属构成的合金等：金、银、铜、铂、锌、铁、铅、锡、铝、钴、铟、镍、铬、钛、锑、铋、锗及镉等金属以及锡-铅合金、锡-铜合金、锡-银合金、锡-铅-银合金及碳化钨等。其中，优选为镍、铜、银或金。用于形成上述芯物质的金属可以与用于形成上述导电部的金属相同，也可以不同。用于形成上述芯物质的金属优选含有用于形成上述导电部的金属。用于形成上述芯物质的金属优选含有镍。用于形成上述芯物质的金属优选含有镍。
上述芯物质的形状没有特别限定。芯物质的形状优选为块状。作为芯物质，例如可举出：粒子状的块、多个微小粒子凝聚而成的凝聚块及无定形块等。
上述芯物质的平均直径(平均粒径)优选为0.001μm以上，更优选为0.05μm以上，优选为0.9μm以下，更优选为0.2μm以下。若上述芯物质的平均直径为上述下限以上及上述上限以下，则有效地降低电极间的连接电阻。
上述芯物质的“平均直径(平均粒径)”表示数均直径(数均粒径)。芯物质的平均直径通过利用电子显微镜或光学显微镜观察50个任意芯物质并算出平均值而求得。
[绝缘性物质]
本发明的导电性粒子优选具备配置于上述导电部外表面上的绝缘性物质。在该情况下，当将导电性粒子用于对电极间进行连接时，可防止邻接的电极间短路。具体而言，多个导电性粒子接触时，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短路而不是上下的电极间的短路。此外，进行电极间连接时，通过利用两个电极对导电性粒子进行加压，可容易地排除导电性粒子的导电部和电极之间的绝缘性物质。导电部在外表面上具有多个突起，因此，可容易地排除导电性粒子的导电部和电极之间的绝缘性物质。
在进行电极间的压接时可更进一步容易地排除上述绝缘性物质，因此，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)丙烯酸聚合物、(甲基)丙烯酸共聚物、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。
作为上述聚烯烃类，可举出：聚乙烯、乙烯-乙酸乙烯酯共聚物及乙烯-丙烯酸酯共聚物等。作为上述(甲基)丙烯酸酯聚合物，可举出聚(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。作为上述嵌段聚合物，可举出：聚苯乙烯、苯乙烯-丙烯酸酯共聚物、SB型苯乙烯-丁二烯嵌段共聚物及SBS型苯乙烯-丁二烯嵌段共聚物以及它们的氢化物等。作为上述热塑性树脂，可举出乙烯基聚合物及乙烯基共聚物等。作为上述热固化性树脂，可举出环氧树脂、酚醛树脂及三聚氰胺树脂等。作为上述水溶性树脂，可举出：聚乙烯醇、聚丙烯酸、聚丙烯酰胺、聚乙烯吡咯烷酮、聚氧乙烯及甲基纤维素等。其中，优选为水溶性树脂，更优选为聚乙烯醇。
作为在上述导电部的表面上配置绝缘性物质的方法，可举出化学的方法及物理的或机械性的方法等。作为上述化学的方法，例如，可举出界面聚合法、粒子存在下的悬浮聚合法及乳液聚合法等。作为上述物理的或机械的方法，可举出：喷雾干燥法、混合法(ハイブリダイゼーション)、静电附着法、喷雾法、浸渍法及真空蒸镀的方法等。其中，绝缘性物质不易脱离，因此，优选在上述导电部的表面上经由化学键合配置上述绝缘性物质的方法。
上述导电部的外表面及绝缘性粒子的表面可以分别由具有反应性官能团的化合物包覆。导电部的外表面和绝缘性粒子的表面可以不进行直接化学键合，可以利用具有反应性官能团的化合物间接性地进行化学键合。可以在导电部的外表面导入羧基后，该羧基经由聚乙烯亚胺等的高分子电解质与绝缘性粒子表面的官能团进行化学键合。
上述绝缘性物质的平均直径(平均粒径)可根据导电性粒子的粒径及导电性粒子的用途等适当选择。上述绝缘性物质的平均直径(平均粒径)优选为0.005μm以上，更优选为0.01μm以上，优选为1μm以下，更优选为0.5μm以下。若绝缘性物质的平均直径为上述下限以上，则导电性粒子分散于粘合剂树脂中时，多个导电性粒子中的导电部彼此不易接触。若绝缘性粒子的平均直径为上述上限以下，则在进行电极间的连接时，排除电极和导电性粒子之间的绝缘性物质，因此，不需要使过高的压力，也不需要加热至高温。
上述绝缘性物质的“平均直径(平均粒径)”表示数平均直径(数均粒径)。绝缘性物质的平均直径使用粒度分布测定装置等求得。
(导电材料)
本发明的导电材料含有上述导电性粒子和粘合剂树脂。上述导电性粒子优选分散于粘合剂树脂中使用，且优选分散于粘合剂树脂中并作为导电材料使用。上述导电材料优选为各向异性导电材料。上述导电材料优选用于对电极间进行电连接。上述导电材料优选为电路连接材料。
上述粘合剂树脂没有特别限定。作为上述粘合剂树脂，可使用公知的绝缘性的树脂。
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。上述粘合剂树脂也可以单独使用一种，也可以组合使用两种以上。
作为上述乙烯基树脂，例如可举出：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-乙酸乙烯酯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。此外，上述固化性树脂也可以是常温固化型树脂、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以与固化剂组合使用。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-丁二烯共聚合橡胶及丙烯腈-苯乙烯嵌段共聚合橡胶等。
上述导电材料除了含有上述导电性粒子及上述粘合剂树脂之外，也可以含有例如：充填剂、增量剂、软化剂、可塑剂、聚合催化剂、固化催化剂、着色剂、氧化防止剂、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。
本发明的导电材料可作为导电糊剂及导电膜等使用。在本发明的导电材料为导电膜的情况下，可以在含有导电性粒子的导电膜上叠层不含有导电性粒子的膜。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，进一步优选为50重量％以上，特别优选为70重量％以上，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地配置在电极间，通过导电材料连接的连接对象部件的连接可靠性更进一步提高。
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，优选为40重量％以下，更优选为20重量％以下，进一步优选为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更进一步提高。
(连接结构体)
通过使用上述导电性粒子或使用含有上述导电性粒子和粘合剂树脂的导电材料，对连接对象部件进行连接，可以得到连接结构体。
优选上述连接结构体是具备：第一连接对象部件、第二连接对象部件、连接第一连接对象部件和第二连接对象部件的连接部，该连接部由上述的导电性粒子形成，或者由含有上述导电性粒子和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，第一连接对象部件、第二连接对象部件由导电性粒子连接。
图4以剖面图示意性地表示使用有本发明第一实施方式的导电性粒子的连接结构体。
图4所示的连接结构体51具备：第一连接对象部件52、第二连接对象部件53、连接第一连接对象部件52和第二连接对象部件53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。连接部54含有导电性粒子1和粘合剂树脂54a。此外，图4中，为了便于图示，概略性地对导电性粒子1进行图示。不仅可以使用导电性粒子1，还可以使用导电性粒子1A、导电性粒子1B等。
第一连接对象部件52在表面(上表面)上具有多个第一电极52a。第二连接对象部件53在表面(下表面)上具有多个第二电极53a。第一电极52a和第二电极53a利用1个或多个导电性粒子1进行电连接。因此，第一连接对象部件52和第二连接对象部件53通过导电性粒子1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个例子可举出如下方法：在第一连接对象部件和第二连接对象部件之间配置上述导电材料，得到叠层体后，对该叠层体进行加热及加压等。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。用于对挠性印刷基板的电极、配置于树脂膜上的电极及触摸面板的电极进行连接的上述加压压力为9.8×104～1.0×106Pa左右。
作为上述连接对象部件，具体而言，可举出：半导体芯片、电容器及二极管等电子部件以及印刷基板、挠性印刷基板、玻璃环氧基板及玻璃基板等的电路基板等电子部件等。上述连接对象部件优选为电子部件。上述导电性粒子优选用于电子部件的电极的电连接。
作为设于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、银电极、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刷基板的情况下，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。此外，在上述电极为铝电极的情况下，可以是仅由铝形成的电极，也可以是将铝层叠层在金属氧化物层的表面上形成的电极。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。
以下，列举实施例及比较例具体地说明本发明。本发明不仅限定于以下的实施例。
(实施例1)
(1)导电性粒子的制备
作为基材粒子A，准备粒径为3.0μm的二乙烯基苯共聚物树脂粒子(积水化学工业株式会社制造“MicroPearlSP-203”)。
使用超声波分散器使上述树脂粒子10重量份分散于含有5重量％的钯催化剂液的碱溶液100重量份中后，过滤溶液，由此，取出树脂粒子。接着，将树脂粒子添加至二甲胺硼烷1重量％溶液100重量份中，使树脂粒子的表面活性化。对表面被活性化的树脂粒子进行充分水洗后，添加至500重量份蒸馏水中使之分散，由此，得到悬浮液。
将悬浮液放入硫酸镍0.09mol/L、硝酸铊30ppm及硝酸铋20ppm的溶液中，得到粒子混合液(A)。
另外，还准备含有硫酸镍0.23mol/L、二甲胺硼烷0.92mol/L、柠檬酸钠0.25mol/L、钨酸钠0.05mol/L、硝酸铊140ppm及硝酸铋30ppm的镍镀液(B)(pH8.0)。
向调整成40℃的分散状态的粒子混合液(A)中缓慢滴加上述镀镍液(B)，进行非电解镀镍。镍镀液(B)的滴加速度设定成10ml/分钟。镀镍液(B)的滴加中，一边通过超声波搅拌使产生的Ni突起核分散，一边进行镀镍。
然后，通过过滤悬浮液而取出粒子，进行水洗并干燥，由此，得到导电性粒子，其在树脂粒子表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。
(2)各向异性导电材料的制备
对得到的导电性粒子7重量份、双酚A型苯氧树脂25重量份、芴型环氧树脂4重量份、苯酚酚醛清漆型环氧树脂30重量份、SI-60L(三新化学工业株式会社制造)进行配合，脱泡搅拌3分钟，由此，得到各向异性导电糊剂。
(3)连接结构体的制备
准备上表面形成有L/S为10μm/20μm的IZO电极图案(第一电极，电极表面的金属的维氏硬度100Hv)的透明玻璃基板。另外，准备在下表面形成有L/S为10μm/20μm的Au电极图案(第二电极，电极表面的金属的维氏硬度50Hv)的半导体芯片。
(实施例2)
除了将镀镍液(B)中的硫酸镍浓度0.23mol/L变更成0.46mol/L以外，与实施例1一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.2μm)且外表面为具有突起的导电层。
使用得到的导电性粒子，与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例3)
除了将镀镍液(B)的pH从8.0变更成6.0以外，与实施例1一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子，与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例4)
除了将上述镀镍液(B)的滴加速度变更成1/2的速度以外，与实施例1一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例5)
除了将上述镀镍液(B)中的硝酸铊140ppm变更成二氧化五钒200ppm以外，与实施例1一样，制备导电性粒子。这样得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例6)
使用超声波分散器使上述树脂粒子10重量份分散于含有5重量％的钯催化剂液的碱溶液100重量份中后，过滤溶液，由此，取出树脂粒子。接着，将树脂粒子添加至二甲胺硼烷1重量％溶液100重量份中，使树脂粒子的表面活性化。对表面被活性化的树脂粒子进行充分水洗后，添加至500重量份蒸馏水中使之分散，由此，得到悬浮液。
将悬浮液放入硫酸镍0.09mol/L、硝酸铊30ppm及硝酸铋20ppm的溶液中，得到粒子混合液(A)。
另外，准备含有硫酸镍0.23mol/L、二甲胺硼烷0.92mol/L、柠檬酸钠0.25mol/L、钨酸钠0.05mol/L、硝酸铊140ppm及硝酸铋30ppm的镀镍液(B)(pH8.0)。
另外，准备含有二甲胺硼烷2.0mol/L、氢氧化钠0.05mol/L的突起形成用镀液(C)(pH10.0)。
向调整成40℃的分散状态的粒子混合液(A)中缓慢滴加上述镀镍液(B)，进行非电解镀镍。镀镍液(B)的滴加速度设定成10ml/分钟。镀镍液(B)的滴加中，一边通过超声波搅拌对产生的Ni突起核进行分散，一边进行镀镍。然后，为了在导电层上形成突起，缓慢滴加突起形成用镀液(C)，而形成突起。突起形成用镀液(C)的滴加速度设定成2ml/分钟。突起形成用镀液(C)的滴加中，一边通过超声波搅拌对产生的Ni突起核进行分散，一边进行镀镍。
然后，通过过滤悬浮液而取出粒子，并进行水洗干燥，由此，得到在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层的导电性粒子。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例7)
基材粒子B除了仅粒径变更成粒径为2.5μm与基材粒子A不同以外，与实施例6一样，得到导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例8)
基材粒子C除了仅粒径变更成粒径为10.0μm与基材粒子A不同以外，与实施例6一样，得到导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例9)
如下得到核壳型有机无机杂化粒子(基材粒子D)：采用基于溶胶凝胶反应的缩合反应，粒径为2.0μm的二乙烯基苯共聚物树脂粒子(积水化学工业株式会社制造“MicroPearlSP-202”)的表面被二氧化硅壳(厚度250nm)包覆。除了将上述基材粒子A变更成上述基材粒子D以外，与实施例6一样，得到导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例10)
向安装有搅拌机及温度计的500mL的反应容器内放入0.13重量％的氨水溶液300g。接着，向反应容器内的氨水溶液中缓慢添加甲基三甲氧基硅烷4.1g、乙烯基三甲氧基硅烷19.2g、聚烷氧基硅氧烷低聚物(信越化学工业株式会社制造“X-41-1053”)0.7g的混合物。一边搅拌，一边进行水解及缩合反应后，添加2.4mL的25重量％氨水溶液，之后从氨水溶液中离析粒子，将得到的粒子以氧分压10-17atm、350℃烧成2小时，得到粒径为2.5μm的有机无机杂化粒子(基材粒子E)。除了将上述基材粒子A变更成上述基材粒子E以外，与实施例6一样，得到导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例11)
在安装有四口可分离式盖、搅拌翼、三通阀、冷却管及温度探针的1000mL的分离式烧瓶中，称取含有甲基丙烯酸甲酯100mmol、N,N,N-三甲基-N-2-甲基丙烯酰氧乙基氯化铵1mmol、2,2’-偶氮二(2-脒基丙烷)二盐酸盐1mmol的单体组合物，使得在离子交换水中固体成分为5重量％，然后，以200rpm进行搅拌，且在氮氛围下以70℃进行24小时聚合。反应结束后，进行冻结干燥，得到表面具有铵基且平均粒径为220nm及CV值为10％的绝缘性粒子。
使绝缘性粒子在超声波照射下分散于离子交换水中，得到绝缘性粒子的10重量％水分散液。
使在实施例6中得到的导电性粒子10g分散于离子交换水500mL中，添加4g绝缘性粒子的水分散液，在室温下搅拌6小时。利用3μm筛网过滤器过滤后，进一步利用甲醇净洗并干燥，得到附着有绝缘性粒子的导电性粒子。
利用扫描电子显微镜(SEM)进行观察，结果，在导电性粒子的表面上仅形成一层绝缘性粒子的包覆层。通过图像解析算出绝缘性粒子的相对于距离导电性粒子的中心2.7μm处面积的包覆面积(即绝缘性粒子的粒径的投影面积)，结果，包覆率为30％。
使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例12)
除了将镀镍液(B)中的柠檬酸钠0.25mol/L变更成丙二酸二钠0.5mol/L以外，与实施例6一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(实施例13)
除了将镀镍液(B)中的柠檬酸钠0.25mol/L变更成丙酸钠1.0mol/L以外，与实施例6一样，制备导电性粒子。如上所述得到导电性粒子，在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(比较例1)
除了将镀镍液(B)中的二甲胺硼烷0.92mol/L变更成次亚磷酸钠1.38mol/L以及将突起形成用镀液(C)二甲胺硼烷2.0mol/L变更成次亚磷酸钠2.18mol/L以及将镀镍液(B)中的柠檬酸钠0.25mol/L变更成酒石酸钠0.3mol/L以外，与实施例6一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-磷导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(比较例2)
除了滴加突起形成用镀液(C)而不进行超声波搅拌以外，与实施例6一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-硼导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(比较例3)
使用金属镍粒子浆料(三井金属株式会社制造“2020SUS”，平均粒径150nm)，在实施例1中使用的树脂粒子的表面上附着金属镍粒子后，形成导电层，且在导电部的外表面上形成突起，以及将镀镍液(B)中的二甲胺硼烷0.92mol/L变更成次亚磷酸钠1.38mol/L，以及将突起形成用镀液(C)二甲胺硼烷2.0mol/L变更成次亚磷酸钠2.18mol/L，除此以外，导电层与实施例6一样地形成，而制备外表面为具有突起的导电层的导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-磷导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
(比较例4)
将镀镍液(B)中的二甲胺硼烷0.92mol/L变更成次亚磷酸钠1.38mol/L，以及将突起形成用镀液(C)二甲胺硼烷2.0mol/L变更成次亚磷酸钠2.18mol/L，以及将镀镍液(B)中的柠檬酸钠0.25mol/L变更成丙酸钠1.0mol/L，除此以外，与实施例6一样，制备导电性粒子。如上所述得到导电性粒子，其在树脂粒子的表面上配置镍-磷导电层(厚度0.1μm)且外表面为具有突起的导电层。使用得到的导电性粒子与实施例1一样，制备各向异性导电材料及连接结构体。
此外，上述实施例和比较例中，全部突起的高度为导电性粒子的粒径的1/15以上、1/6以下。
(评价)
(1)微晶尺寸
使用X射线衍射装置(理学电机株式会社制造“RINT2500VHF”)，在管电压40kV、管电流50mA、X射线：CuKα线及波长λ：的条件下，测定导电部中的微晶尺寸。
(2)晶格应变
使用X射线衍射装置(理学电机株式会社制造“RINT2500VHF”)，在管电压40kV、管电流50mA、X射线：CuKα线及波长λ：的条件下，测定导电部的晶格应变。
(3)突起的状态
使用扫描电子显微镜(SEM)，将图像倍率设定成25000倍，任意选择10个导电性粒子，并观察各个导电性粒子的突起部。对于全部突起部，评价在金属或金属合金的粒子间是否观察到晶界，并分类成由金属或金属合金形成且多个金属或金属的合金粒子不会连结成列状的突起部(第一突起部)，和由多个金属或金属合金的粒子连结成列状的粒子连结体形成的突起部(第二突起部)。如上所述，测量每个导电性粒子的1)第一突起部的个数和2)第二突起部的个数。算出第一突起部和第二突起部的总个数100％中第一突起部的比例和第二突起部的比例。
(4)晶体结构的确认(连续性)
使用场发射透射电子显微镜(FE-TEM)(日本电子株式会社制造“JEM-ARM200F”)，在500万倍下评价是否在外表面上具有多个突起的导电部的晶界。另外，评价在导电部的具有突起的部分和不具有突起的部分，晶体结构是否连续。
(5)导电性粒子的压缩弹性模量(10％K值)
在23℃的条件下，通过上述方法并使用微小压缩试验机(Fischer株式会社制造“FischerscopeH-100”)测定导电性粒子的10％K值。
(6)电极间的连接电阻
通过四端子法分别测定得到的连接结构体的上下的电极间的连接电阻。算出两个连接电阻的平均值。此外，通过根据电压＝电流×电阻的关系，测定流过恒定电流时的电压，从而可以求得连接电阻。根据下述基准判定电极间的连接电阻。
[电极间的连接电阻的判定基准]
○○○：连接电阻为2.0Ω以下
○○：连接电阻超过2.0Ω且3.0Ω以下
○：连接电阻超过3.0Ω且5.0Ω以下
△：连接电阻超过5.0Ω且10Ω以下
×：连接电阻超过10Ω
(7)突起的高度
使用扫描电子显微镜(SEM)，将图像倍率设定成25000倍，任意选择10个导电性粒子，观察各个导电性粒子的突起部。测量得到的导电性粒子中的突起部的高度。
将结果示于下述表1中。

Claims (11)

1.一种导电性粒子，其具备：
基材粒子以及配置于所述基材粒子表面上的导电部，
所述导电部在外表面具有多个突起，
所述导电部具有晶体结构，
在所述导电部的具有所述突起的部分和不具有所述突起的部分，晶体结构是连续的。
2.如权利要求1所述的导电性粒子，其中，
所述导电部由金属或金属合金形成，
所述突起具有多个第一突起部，所述第一突起部由所述金属或金属合金形成，而不是由多个所述金属或金属合金的粒子连结成列状而形成，
所述突起不具有由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部，或者具有至少一个由多个所述金属或金属合金的粒子连接成列状而得到的粒子连结体所形成的第二突起部，
所述第一突起部和所述第二突起部的总个数100％中的70％以上为所述第一突起部。
3.如权利要求2所述的导电性粒子，其中，
所述第一突起部和所述第二突起部的总个数100％中的90％以上为所述第一突起部。
4.如权利要求1～3中任一项所述的导电性粒子，其中，
所述导电部中的微晶尺寸为0.1nm以上、100nm以下。
5.如权利要求1～4中任一项所述的导电性粒子，其中，
所述导电部的晶格应变为0.001％以上、且10％以下。
6.如权利要求1～5中任一项所述的导电性粒子，其中，
所述导电部含有镍。
7.如权利要求1～6中任一项所述的导电性粒子，其中，
在所述导电部的内部及内侧不具有用于使所述导电部的外表面隆起的芯物质。
8.如权利要求1～7中任一项所述的导电性粒子，其中，
所述突起的高度为所述导电性粒子的粒径的1/100以上。
9.如权利要求1～8中任一项所述的导电性粒子，其具备配置于所述导电部外表面上的绝缘性物质。
10.一种导电材料，其含有权利要求1～9中任一项所述的导电性粒子和粘合剂树脂。
11.一种连接结构体，其具备：
第一连接对象部件，其表面具有第一电极；
第二连接对象部件，其表面具有第二电极；
连接部，其将所述第一连接对象部件和所述第二连接对象部件连接在一起，
所述连接部由权利要求1～9中任一项所述的导电性粒子形成，或者由含有所述导电性粒子和粘合剂树脂的导电材料形成，
所述第一电极和所述第二电极通过所述导电性粒子实现了电连接。
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