CN112272851A - 导电性糊料和烧结体 - Google Patents

导电性糊料和烧结体 Download PDF

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Publication number
CN112272851A
CN112272851A CN201980039267.2A CN201980039267A CN112272851A CN 112272851 A CN112272851 A CN 112272851A CN 201980039267 A CN201980039267 A CN 201980039267A CN 112272851 A CN112272851 A CN 112272851A
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silver powder
mass
parts
median diameter
conductive paste
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CN201980039267.2A
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CN112272851B (zh
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酒金婷
竹政哲
清野顺子
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Senju Metal Industry Co Ltd
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Senju Metal Industry 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
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    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
    • B22F1/107—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material containing organic material comprising solvents, e.g. for slip casting
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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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    • B22F3/10—Sintering only
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    • B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
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Abstract

本发明的目的在于，提供制成烧结体时的电阻值低、导电性优异的导电性糊料和其烧结体。导电性糊料，其包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份。

Description

导电性糊料和烧结体
技术领域
本发明涉及导电性糊料和烧结体。
背景技术
以往，使用μm尺寸(以下有时称为“微米尺寸”)或nm尺寸(以下有时称为“纳米尺寸”)的金属粉的导电性糊料广泛用作导电性材料。使用这样的微米尺寸或纳米尺寸的金属粉的导电性糊料用于例如印刷电路板中的电极、配线等电子电路的形成；电子基板与电子部件之间的接合。
作为使用这样的金属粉的导电性糊料，专利文献1中提出了糊状银颗粒组合物，其特征在于，其为包含平均粒径为0.1~18μm、碳量为1.0重量%以下的非球状银颗粒、和挥发性分散介质的糊状物，通过加热，该挥发性分散介质挥散，该非球状银颗粒彼此烧结。专利文献1中，作为上述非球状银颗粒，具体公开了使用薄片状银颗粒的导电性糊料。然而，如本申请的比较例2中后述那样，如专利文献1中记载的仅使用18μm以下的小平均粒径的银颗粒(银粉)的导电性糊料烧结而制成配线时的电阻值高，导电性不充分。
此外，专利文献2中提出了导电性糊料，其包含具有0.1μm~15μm的平均粒径(中位直径)的银颗粒和醇。专利文献2中，作为上述银颗粒，具体公开了将平均粒径(中位直径)为0.3μm的银颗粒和平均粒径(中位直径)为2.0~3.2μm的银颗粒的2种混合而得到的导电性糊料。然而，如本申请的比较例3和4中后述那样，如专利文献2中记载的仅混合15μm以下的小平均粒径的2种银颗粒(银粉)的导电性糊料烧结而制成配线时的电阻值高，导电性不充分。
专利文献3中，提出了以银粉末作为主体的导体糊料的制造方法，包括：准备将平均粒径彼此不同的至少2种球状银粉末、和平均粒径彼此不同的至少2种薄片状银粉末混合而成的导电性粉末的步骤；和，使前述导电性粉末分散在有机媒介中的步骤。专利文献3中还公开了作为上述至少2种球状银粉末和至少2种薄片状银粉末，使用平均粒径0.1~0.8μm的球状银粉末、平均粒径1.0~2.0μm的球状银粉末、平均粒径1~4μm的薄片状银粉末、和平均粒径5~15μm的薄片状银粉末的组合。然而，专利文献3中记载的4种银粉末均具有15μm以下的小平均粒径。如本申请的比较例11~13中后述那样，如专利文献3中记载的不含具有25μm以上的中位直径的银粉的导电性糊料，将电子基板与电子部件接合时的接合强度不充分。
专利文献4中提出了导电性粘接剂，其特征在于，包含将银箔粉碎而得到的平均粒径45μm~1000μm且褶皱状的银粉的表观密度0.01g/cm3~0.1g/cm3的膨松银粉的填充量为5重量%以上且低于25重量%，粘接剂的填充量大于75重量%且为95重量%以下。然而，专利文献4中记载的导电性粘接剂是以含有高分子化合物为前提，是与仅将银粉和溶剂混合而得到的导电性糊料不同的材料。
现有技术文献
专利文献
专利文献1：国际公开第2007/034833号
专利文献2：日本特开2009-170277号
专利文献3：日本特开2004-362950号
专利文献4：日本特开平5-81923号。
以往的导电性糊料存在的问题在于，在印刷电路板上涂布后烧结而制成配线时的电阻值高，导电性不充分，此外，将电子基板与电子部件接合时的接合强度也不充分。
因此，期望制成烧结体时的电阻值低、导电性优异的导电性糊料。进一步，除了优异的导电性之外，还期望接合电子基板等时的接合强度优异的导电性糊料。
发明内容
发明要解决的课题
本发明的目的在于，提供制成烧结体时的电阻值低、导电性优异的导电性糊料和其烧结体。此外，本发明的另一目的还在于，提供除了优异的导电性以外接合电子基板等时的接合强度也优异的导电性糊料和其烧结体。
用于解决课题的手段
本发明人等为了解决上述课题而进行了深入研究，结果发现通过组合使用特定量的具有15μm以下的中位直径D50的薄片状银粉、特定量的具有25μm以上的中位直径D50的银粉和溶剂，能够解决上述课题，从而完成了本发明。本发明的具体的方式如下所述。
应予说明，本说明书中，使用“~”表示数值范围时，其范围包括两端的数值。
[1]导电性糊料，其包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，
相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份。
[2]导电性糊料，其包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉、具有在0.1μm~0.5μm与1μm~15μm具有峰的双峰性的粒度分布的银粉、和溶剂，
相对于前述薄片状银粉、前述具有25μm以上的中位直径D50的银粉、和前述具有双峰性的粒度分布的银粉的总计100质量份，前述薄片状银粉的含量为8~55质量份，前述具有25μm以上的中位直径D50的银粉的含量为15~65质量份，前述具有双峰性的粒度分布的银粉的含量为4~45质量份。
[3]根据[1]所述的导电性糊料，其特征在于，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为30~42质量份，前述具有25μm以上的中位直径D50的银粉的含量为58~70质量份。
[4]根据[2]所述的导电性糊料，其特征在于，相对于前述薄片状银粉、前述具有25μm以上的中位直径D50的银粉、和前述具有双峰性的粒度分布的银粉的总计100质量份，前述薄片状银粉的含量为23~35质量份，前述具有25μm以上的中位直径D50的银粉的含量为40~63质量份，前述具有双峰性的粒度分布的银粉的含量为12~35质量份。
[5]烧结体，其是将[1]~[4]中任一项所述的导电性糊料烧结而成。
[6]烧结体，其是将包含基板、[1]~[4]中任一项所述的导电性糊料和导电体的层叠体烧结而成。
发明的效果
本发明的导电性糊料和其烧结体制成烧结体时的电阻值低，导电性优异。
此外，本发明的导电性糊料和烧结体除了优异的导电性之外，接合电子基板等时的接合强度也优异。
附图说明
图1是实施例中的电阻值的评价中使用的配线的示意图。
图2是实施例中的剪切强度的评价中使用的试样的示意图。
图3A是通过扫描型电子显微镜(倍率：1000倍)拍摄实施例中的银粉(2-1)的表面而得到的图像。
图3B是通过扫描型电子显微镜(倍率：1000倍)拍摄实施例中的银粉(2-2)的表面而得到的图像。
图3C是通过扫描型电子显微镜(倍率：1000倍)拍摄实施例中的银粉(2-3)的表面而得到的图像。
图3D是通过扫描型电子显微镜(倍率：20000倍)拍摄实施例中的银粉(2-4)的表面而得到的图像。
图4A是通过扫描型电子显微镜(倍率：1000倍)拍摄利用实施例3的烧结体的配线的表面而得到的图像。
图4B是通过扫描型电子显微镜(倍率：700倍)拍摄利用实施例3的烧结体的配线的截面而得到的图像。
图4C是通过扫描型电子显微镜(倍率：5000倍)拍摄利用实施例3的烧结体的配线的表面而得到的图像。
图4D是通过扫描型电子显微镜(倍率：10000倍)拍摄利用实施例3的烧结体的配线的表面而得到的图像。
图5A是通过扫描型电子显微镜(倍率：1000倍)拍摄利用比较例3的烧结体的配线的表面而得到的图像。
图5B是通过扫描型电子显微镜(倍率：700倍)拍摄利用比较例3的烧结体的配线的截面而得到的图像。
图5C是通过扫描型电子显微镜(倍率：5000倍)拍摄利用比较例3的烧结体的配线的表面而得到的图像。
图5D是通过扫描型电子显微镜(倍率：10000倍)拍摄利用比较例3的烧结体的配线的表面而得到的图像。
图6A是通过扫描型电子显微镜(倍率：400倍)拍摄利用比较例7的烧结体的配线的表面而得到的图像。
图6B是通过扫描型电子显微镜(倍率：1000倍)拍摄利用比较例7的烧结体的配线的表面而得到的图像。
图7A是通过扫描型电子显微镜(倍率：1000倍)拍摄实施例3的烧结后的剪切强度测定用试样的截面而得到的图像。
图7B是通过扫描型电子显微镜(倍率：2500倍)拍摄实施例3的烧结后的剪切强度测定用试样的截面而得到的图像。
图8A是通过扫描型电子显微镜(倍率：1000倍)拍摄比较例3的烧结后的剪切强度测定用试样的截面而得到的图像。
图8B是通过扫描型电子显微镜(倍率：2500倍)拍摄比较例3的烧结后的剪切强度测定用试样的截面而得到的图像。
具体实施方式
以下，针对本发明的导电性糊料和烧结体进行说明。
[第一实施方式]
本发明的导电性糊料包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份。
薄片状银粉的中位直径D50为15μm以下、优选为0.1μm~15μm、更优选为2μm~10μm。如果薄片状银粉的中位直径D50为上述数值范围内，则与使用球状粉的情况相比表面积增加，因此容易形成烧结体。
本发明中，各银粉的中位直径D50是指使用SALD-2300(岛津制作所制)，通过激光衍射法测定得到的值。
本发明中，对于薄片状银粉，构成该银粉的颗粒的过半数在显微镜下确认为薄片状(薄片状或剥片状)即可。典型地，是指构成该银粉的颗粒(一次颗粒)的51质量%以上具有薄片(薄片或剥片)形状。在此，薄片状(薄片状或剥片状)的颗粒是指长宽比(最长的长径/最短的短径之比)为5~300的颗粒。
具有25μm以上的中位直径D50的银粉的中位直径D50为25μm以上、优选为25μm~100μm、更优选为30μm~80μm。
在仅使用低于25μm的粒径的情况下，电流在各颗粒中传递流动，因此颗粒的接点数变多，整体的电阻率变高。另一方面，如果具有25μm以上的中位直径D50的银粉的中位直径为上述数值范围内，则包含1粒大的颗粒，因此能够减少颗粒的接点数，整体的电阻率变低。因此，与仅使用低于25μm的粒径的情况相比，得到制成烧结体时的电阻值低、导电性优异的导电性糊料。
具有25μm以上的中位直径D50的银粉的形状没有特别限定，可以为球状和非球状中任一者。作为非球状的例子，可以举出薄片状、针状、角状、树枝状、粒状、不规则形状、泪滴状、板状、极薄板状、六角板状、柱状、棒状、多孔状、纤维状、块状、海绵状、倾斜角状、圆形等。这样的形状之中，优选球状、柱状。
薄片状银粉相对于薄片状银粉与具有25μm以上的中位直径D50的银粉的总计100质量份的含量为15~70质量份、优选为30~60质量份、更优选为30~50质量份。
具有25μm以上的中位直径D50的银粉相对于薄片状银粉与具有25μm以上的中位直径D50的银粉的总计100质量份的含量为30~85质量份、优选为40~70质量份、更优选为50~70质量份。
如果薄片状银粉的含量和具有25μm以上的中位直径D50的银粉的含量均为上述数值范围内，则得到制成烧结体时的电阻值低、导电性优异、而且接合电子基板等时的接合强度优异的导电性糊料。
薄片状银粉相对于导电性糊料100质量份的含量优选为10~50质量份、更优选为20~50质量份、最优选为30~50质量份。
如果薄片状银粉相对于导电性糊料100质量份的含量低于10质量份，则难以将包含薄片状银粉的组合物制成糊料状。此外，即使能够将包含薄片状银粉的组合物制成糊料状，由这样的导电性糊料得到的烧结体的电阻值也变高，导电性差。
具有25μm以上的中位直径D50的银粉相对于导电性糊料100质量份的含量优选为15~60质量份、更优选为20~55质量份、最优选为30~55质量份。如果具有25μm以上的中位直径D50的银粉的含量为上述数值范围内，则得到制成烧结体时的电阻值低、导电性优异、而且接合电子基板等时的接合强度优异的导电性糊料。
作为溶剂，可以举出水、醇系溶剂、二醇醚系溶剂、萜品醇类等。
作为醇系溶剂，可以举出异丙醇、1,2-丁二醇、异冰片基环己醇、2,4-二乙基-1,5-戊二醇、2,2-二甲基-1,3-丙二醇、2,5-二甲基-2,5-己二醇、2,5-二甲基-3-己炔-2,5-二醇、2,3-二甲基-2,3-丁二醇、1,1,1-三(羟基甲基)乙烷、2-乙基-2-羟基甲基-1,3-丙二醇、2,2'-氧基双(亚甲基)双(2-乙基-1,3-丙二醇)、2,2-双(羟基甲基)-1,3-丙二醇、1,2,6-三羟基己烷、双[2,2,2-三(羟基甲基)乙基]醚、1-乙炔基-1-环己醇、1,4-环己二醇、1,4-环己烷二甲醇、赤藓糖醇、苏糖醇、愈创木酚甘油醚、3,6-二甲基-4-辛炔-3,6-二醇、2,4,7,9-四甲基-5-癸炔-4,7-二醇等。
作为二醇醚系溶剂，可以举出二乙二醇单-2-乙基己基醚、乙二醇单苯基醚、2-甲基戊烷-2,4-二醇、二乙二醇单己基醚、二乙二醇二丁基醚、三乙二醇单丁基醚等。
溶剂相对于导电性糊料100质量份的含量优选为2~20质量份、更优选为2~15质量份、最优选为5~10质量份。通过溶剂的含量为上述数值范围内，能够得到涂布性良好的糊料。
[第二实施方式]
本发明的导电性糊料包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉、具有在0.1μm~0.5μm与1μm~15μm具有峰的双峰性的粒度分布的银粉和溶剂，相对于前述薄片状银粉、前述具有25μm以上的中位直径D50的银粉、和前述具有双峰性的粒度分布的银粉的总计100质量份，前述薄片状银粉的含量为8~55质量份，前述具有25μm以上的中位直径D50的银粉的含量为15~65质量份，前述具有双峰性的粒度分布的银粉的含量为4~45质量份。
作为薄片状银粉的中位直径D50、薄片形状的定义、薄片状银粉相对于导电性糊料100质量份的含量、具有25μm以上的中位直径D50的银粉的中位直径D50和形状、具有25μm以上的中位直径D50的银粉相对于导电性糊料100质量份的含量、溶剂的种类、以及溶剂相对于导电性糊料100质量份的含量，可以使用第一实施方式中示出的。
具有双峰性的粒度分布的银粉在0.1μm~0.5μm与1μm~15μm具有峰，优选在0.1μm~0.3μm与3μm~10μm具有峰。
本发明中，双峰性的粒度分布是指使用SALD-2300(岛津制作所制)，通过激光衍射法测定得到的值。
具有双峰性的粒度分布的银粉的形状没有特别限定，可以为球状和非球状中任一者。作为非球状的例子，可以举出薄片状、针状、角状、树枝状、粒状、不规则形状、泪滴状、板状、极薄板状、六角板状、柱状、棒状、多孔状、纤维状、块状、海绵状、倾斜角状、圆形等。这样的形状之中，优选球状。
在具有双峰性的粒度分布的银粉的形状为球状的情况下，不限于正球状，构成该银粉的颗粒的过半数在显微镜下确认为球状即可。典型地，是指构成该银粉的颗粒(一次颗粒)的80质量%以上具有球状或与其类似的形状。在此，球状的颗粒是指长宽比(长径/短径的比)为1.0~1.3的颗粒。
薄片状银粉相对于薄片状银粉、具有25μm以上的中位直径D50的银粉、和具有双峰性的粒度分布的银粉的总计100质量份的含量为8~55质量份、优选为15~40质量份、更优选为20~35质量份。
具有25μm以上的中位直径D50的银粉相对于薄片状银粉、具有25μm以上的中位直径D50的银粉、和具有双峰性的粒度分布的银粉的总计100质量份的含量为15~65质量份、优选为20~65质量份、更优选为30~60质量份。
具有双峰性的粒度分布的银粉相对于薄片状银粉、具有25μm以上的中位直径D50的银粉、和具有双峰性的粒度分布的银粉的总计100质量份的含量为4~45质量份、优选为10~40质量份、更优选为15~30质量份。
如果薄片状银粉的含量、具有25μm以上的中位直径D50的银粉的含量、和具有双峰性的粒度分布的银粉的含量均为上述数值范围内，则得到制成烧结体时的电阻值低、导电性优异、而且接合电子基板等时的接合强度优异的导电性糊料。
具有双峰性的粒度分布的银粉相对于导电性糊料100质量份的含量优选为5~40质量份、更优选为10~35质量份、最优选为10~30质量份。
本发明的导电性糊料可以使用薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂、以及根据情况使用具有双峰性的粒度分布的银粉，使用ARV-310(株式会社シンキー制)装置，混炼而制作。
[第三实施方式]
本发明提供烧结体，其是将上述的导电性糊料烧结而成的。
烧结体可以通过在基板上印刷或涂布导电性糊料后，通过烧结而得到。这样的烧结体具有导电性，因此作为基板上的配线(电子电路)而发挥功能。作为印刷或涂布导电性糊料的方法，没有特别限定，可以举出分配涂布、印刷涂布、喷雾涂布、刷涂、注入等。
作为设置有烧结体的基板，没有特别限定，可以举出高耐热的FR4等玻璃纤维强化环氧系印刷基板、聚酰亚胺系的基板、DBA(Direct Bonded Aluminum，直接敷铝)、DBC(Direct Bonded Copper，直接敷铜)等陶瓷基板、铜、银、铝等金属基板、Cu引线框架等。基板上搭载有电子部件。可以对金属基板实施金属镀敷。作为金属镀敷中使用的金属，可以举出金、银、镍、锡等。
将导电性糊料烧结时的条件没有特别限定，烧结中的加热温度优选为150~350℃、更优选为180~300℃、最优选为200~300℃。此外，烧结中的加热时间优选为10~60分钟、更优选为15~45分钟、最优选为20~30分钟。烧结时，对导电性糊料不施加压力。烧结可在大气氛围下或氧气浓度为1%以上的氛围下进行。
作为烧结体的形状，没有特别限定，可以举出片状、膜状、胶带状、线状、圆盘状、块状、点状、不定形等。
本发明的烧结体可以实现8.5μΩ·cm以下的电阻值。烧结体的电阻值可以通过后述的(评价)的“(1)电阻值的评价”中记载的方法测定。
[第四实施方式]
本发明提供烧结体，其是将包含基板、上述的导电性糊料和导电体的层叠体烧结而成的。
可在基板上按顺序层叠导电性糊料和导电体，制造层叠体。并且，通过将该层叠体烧结，可以得到烧结体。这样的烧结体中，源自导电性糊料的部分具有导电性，且将基板与导电体接合，因此作为导电性的接合部(粘接部)而发挥功能。作为接合的基板，可以举出电路基板、玻璃纤维强化环氧系印刷基板、聚酰亚胺系的基板、陶瓷基板、金属基板、Cu引线框架等。此外，作为接合的导电体，可以举出电容器和电阻等芯片部件、在晶片上形成电阻、晶体管、电容器和集成电路等半导体元件后从晶片中切出各半导体元件的区隔而得到的芯片等。
将上述层叠体烧结时的条件根据要接合的对象而不同，例如对Ag镀敷Cu引线框架将4mm×4mm硅芯片烧结的情况下，可以举出在250℃下30分钟、大气压、大气氛围下的条件。
烧结后的上述层叠体可以实现25MPa以上的剪切强度。本发明中，剪切强度是指通过按照JIS Z 3198的方法而测定的剪切强度，烧结后的上述层叠体的接合强度(剪切强度)可以通过后述的(评价)的“(2)剪切强度的评价”中记载的方法测定。
以下，通过实施例具体说明本发明，但本发明不限于实施例中记载的内容。
实施例
(评价)
针对实施例1~11和比较例1~13的各导电性糊料，如以下所示，进行电阻值和剪切强度的评价。
(1)电阻值的评价
将实施例1~11和比较例1~13的各导电性糊料通过使用金属掩模(厚度100μm)的丝网印刷涂布在玻璃基板(厚度2mm)上。将涂布有导电性糊料的玻璃基板在大气氛围下、大气压下，在200℃下加热30分钟，进行烧结，形成配线。以这样的方式得到的利用导电性糊料的烧结体的配线是长×宽的尺寸：3mm×30mm。所得配线的示意图示于图1。
针对以这样的方式得到的实施例1~11和比较例1~13的各利用烧结体的配线，在室温(25℃)和相对湿度50%的条件下，使用标准外侧千分尺M110(株式会社ミツトヨ制)，测定配线的厚度。并且，针对实施例1~11和比较例1~13的各配线，在室温(25℃)和相对湿度50%的条件下，使用lozesta-GP MCP-T610(三菱化学株式会社制)，通过4端子法进行配线的电阻值(μΩ·cm)的测定。作为电阻值的测定中的4端子探针，使用ESP探针(三菱化学株式会社制、MCP-TP08P、No.014052B)。针对各配线进行3次测定，算出电阻值(μΩ·cm)的平均值。
如果配线的电阻值的平均值为8.5μΩ·cm以下，则可以说导电性良好。
(2)剪切强度的评价
准备从铜基板侧按顺序通过溅射而层叠有Ti层(厚度40nm)和Ag层(厚度1000nm)的铜基板(长×宽的尺寸：50mm×50mm)(以下称为试验片(1))。在试验片(1)的Ag层上，将实施例1~11和比较例1~13的各导电性糊料进行使用金属掩模(厚度100μm)的丝网印刷。
另一方面，准备从Si芯片侧按顺序通过溅射而层叠有Ti层(厚度40nm)和Ag层(厚度1000nm)的Si芯片(长×宽的尺寸：3mm×3mm)(以下称为试验片(2))。
并且，针对实施例1~3和5~11、以及比较例1~3和5~13，在涂布于试验片(1)的导电性糊料上，使用芯片安装器(制品名SMT―64RH、奥原电气株式会社制)，层叠试验片(2)的Ag层侧，得到包含试验片(1)、导电性糊料和试验片(2)的试样。将所得试样在大气氛围下、大气压下，在200℃下加热30分钟，进行烧结。针对作为溶剂而使用乙醇的实施例4和比较例4，如果使用芯片安装器，则在导电性糊料上层叠试验片(2)前溶剂挥发，无法接合试验片(2)，此外，如果在大气压下进行烧结，则溶剂的挥发快，因此无法接合试验片(2)。因此，针对实施例4和比较例4，在导电性糊料上的试验片(2)的层叠通过手动而快速进行，将烧结时的压力设为0.4MPa，除此之外的条件与实施例1~3和5~11、以及比较例1~3和5~13相同，得到烧结后的试样。
所得烧结后的试样的示意图示于图2。
并且，针对比较例2、3和10的各烧结后的试样，使用万能型粘接测试器NordsonDAGE Series4000(Noedon Corporation制)，在室温(25℃)条件下，通过按照JIS Z3198的方法，进行试验片(1)与试验片(2)之间的剪切强度(MPa)的测定。针对各试样进行5次测定，算出剪切强度(MPa)的平均值。
如果试样的剪切强度的平均值为25MPa以上，则可以说试验片彼此的接合性良好。
(实施例1~11、比较例1~13)
作为薄片状银粉，使用市售的制品名AgC239(福田金属箔粉工业株式会社制、中位直径D50：2.5μm、薄片状)(以下称为“银粉(1)”)。
此外，具有25μm以上的中位直径D50的2种银粉(以下分别称为“银粉(2-1)”和“银粉(2-2)”)、具有低于25μm的中位直径D50的银粉(以下称为“银粉(2-3)”)、具有300~700nm的粒度分布的银粉(以下称为“银粉(2-4)”)、和具有双峰性的粒度分布的银粉(以下称为“银粉(3)”)通过以下的流程制备。
·银粉(2-1)的制造
通过将银加热而制成熔融状态，将该熔融的银喷雾而冷却的方法(熔融喷雾法)，制作中位直径D50：36.34μm的球状的银粉(银粉(2-1))。
·银粉(2-2)的制造
通过将银加热而制成熔融状态，将该熔融的银喷雾而冷却的方法(熔融喷雾法)，制作中位直径D50：31.13μm的球状的银粉(银粉(2-2))。
·银粉(2-3)的制造
通过将银加热而制成熔融状态，将该熔融的银喷雾而冷却的方法(熔融喷雾法)，制作中位直径D50：13.67μm的球状的银粉(银粉(2-3))。
·银粉(2-4)的制造
通过下述制造方法制作在300~700nm具有峰的银粉(银粉(2-4))。
首先，在50g的乙二醇(多元醇)中溶解硝酸银(银化合物)1.0g。接着，在乙二醇中分散聚乙烯基吡咯烷酮(分散剂)0.5g。接着，使乙二醇升温至150℃(反应温度)后，将反应温度保持150℃，同时在以500rpm的旋转速度搅拌的同时进行1小时反应。将反应后的银粉使用金属网从乙二醇(多元醇)分离，使用乙醇洗涤所分离的银粉，得到银粉(2-4)。
针对所得银粉(2-1)~(2-4)，通过场发射型扫描电子显微镜(FE-SEM)(日本电子制JSM-7000F)拍摄得到的图像示于图3A~3D。图3A~3C分别是对银粉(2-1)~(2-3)的表面以倍率1000倍拍摄而得到的图像，图3D是对银粉(2-4)的表面以倍率20000倍拍摄而得到的图像。
以下，将上述银粉(2-1)~(2-4)总称为银粉(2)。
·银粉(3)的制造
通过下述制造方法制作具有在0.1μm~0.5μm与1μm~15μm具有峰的双峰性的粒度分布的银粉(银粉(3))。
首先，通过与银粉(2-4)完全相同的制作方法制作银粉A。并且，在以500rpm的旋转速度将50g的乙二醇搅拌的同时，在乙二醇中溶解硝酸银2.0g后，进一步在乙二醇中分散0.05g的银粉A。接着，使乙二醇升温至150℃(反应温度)后，将反应温度保持150℃，同时在以500rpm的旋转速度搅拌的同时进行1小时反应。其后，使用金属网将反应后的银粉从乙二醇中分离，使用乙醇洗涤所分离的银粉，得到银粉(3)。
应予说明，本实施例和比较例中使用的银粉(1)和(2-1)~(2-3)的中位直径D50、以及银粉(2-4)和银粉(3)的粒度分布是指使用SALD-2300(岛津制作所制)，通过激光衍射法测定得到的值。
·导电性糊料的制造
以以下的表1和2所示的组成，制备实施例1~11以及比较例1~13的导电性糊料。
应予说明，以下的表1和2中的各成分的数值表示各成分相对于导电性糊料100质量份的质量份。
并且，针对实施例1~11和比较例1~13的导电性糊料，进行上述的电阻值和剪切强度的评价。评价结果示于以下的表1和2。
Figure DEST_PATH_IMAGE001
Figure 805798DEST_PATH_IMAGE002
实施例1~11的导电性糊料包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份。
根据上述表1的结果可知，对于实施例1~11的导电性糊料，利用烧结体的配线的电阻值低，具有良好的导电性，此外，烧结体的剪切强度优异，具有良好的接合性。
可知其中特别是实施例2和3的利用烧结体的配线的电阻值低，具有更良好的导电性，此外，烧结体的剪切强度优异，具有更良好的接合性。实施例2和3的导电性糊料中，相对于薄片状银粉与具有25μm以上的中位直径D50的银粉的总计100质量份，薄片状银粉的含量为30~42质量份，具有25μm以上的中位直径D50的银粉的含量为58~70质量份。
另一方面，上述表2所示的比较例1是不含银粉(1)和银粉(2)的导电性糊料。比较例2~4和10是不含银粉(2)的导电性糊料。此外，比较例7和9是不含银粉(1)的导电性糊料。比较例5和8的导电性糊料包含银粉(1)和银粉(2-1)两者，但相对于银粉(1)和银粉(2-1)的总计100质量份，银粉(1)的含量低于15质量份，银粉(2-1)的含量大于85质量份。此外，比较例6的导电性糊料包含银粉(1)和银粉(2-1)两者，但相对于银粉(1)和银粉(2)的总计100质量份，银粉(1)的含量大于70质量份，银粉(2-1)的含量低于30质量份。比较例11~13是不含中位直径D50为25μm以上的银粉的导电性糊料。
由表2的结果可知，比较例1~5、7~10和13的导电性糊料与实施例1~13的导电性糊料相比，利用烧结体的配线的电阻值高，导电性不充分，此外，烧结体的剪切强度低，接合性差。对于比较例6的导电性糊料，烧结体具有良好的接合性，但利用烧结体的配线的电阻值高，导电性不充分。此外，对于比较例11和12的导电性糊料，利用烧结体的配线具有良好的导电性，但烧结体的剪切强度低，接合性差。
针对实施例3、以及比较例3和7的利用烧结体的配线，通过场发射型扫描电子显微镜(FE-SEM)(日本电子制 JSM-7000F)拍摄得到的图像示于图4A~6B。
图4A、4C和4D是对实施例3的配线的表面各自以倍率1000、5000、10000倍拍摄而得到的图像。图4B是对实施例3的配线的截面以倍率700倍拍摄而得到的图像。
图5A、5C和5D是对比较例3的配线的表面各自以倍率1000、5000、10000倍拍摄而得到的图像。图5B是对比较例3的配线的截面以倍率700倍拍摄而得到的图像。
图6A和6B是对比较例7的配线的表面各自以倍率400、1000倍拍摄而得到的图像。
根据图4A~4D，实施例3的配线中，在烧结体中观察到各自源自直径小且薄片状的银粉(1)、直径大的银粉(2-1)、和直径小且具有双峰性的粒度分布的银粉(3)的结构。并且可知，实施例3的配线中，薄片状的银颗粒和直径小的银颗粒与直径大的银颗粒彼此充分接触，且融合。由此可以认为，实施例3的配线中配线内的电子的移动速度变大，电阻值变低。
另一方面，根据图5A~5D，比较例3的配线中，在烧结体中观察到各自源自直径小且薄片状的银粉(1)、和直径小且具有双峰性的粒度分布的银粉(3)的结构。但是可知，比较例3的配线，仅由直径小的银粉(1)和(3)构成，不含直径大的银粉(2-1)或(2-2)，因此银颗粒彼此部分接触，但在其他部分处，银颗粒彼此未充分接触，未充分融合。由此可以认为，比较例3的配线，与实施例3的配线相比，电阻值变高。
此外，根据图6A和6B可知，比较例7的配线，仅由直径大的银粉(2-1)构成，不含直径小的银粉(1)和(3)，因此银颗粒各自独立存在，银颗粒彼此几乎不融合。由此可以认为，比较例7的配线中，电阻值变得极高。
此外，针对实施例3和比较例3的烧结后的剪切强度测定用试样，通过场发射型扫描电子显微镜(FE-SEM)(日本电子制 JSM-7000F)拍摄得到的图像示于图7A~8B。
图7A和7B是对实施例3的试样的截面各自以倍率1000、2500倍拍摄得到的图像。图8A和8B是对比较例3的试样的截面各自以倍率1000、2500倍拍摄得到的图像。
根据图7A和7B，实施例3的试样中，在烧结体中观察到各自源自直径小且薄片状的银粉(1)、直径大的银粉(2-1)、和直径小且具有双峰性的粒度分布的银粉(3)的结构。并且可知，实施例3的试样中，薄片状的银颗粒和直径小的银颗粒与直径大的银颗粒彼此充分接触和融合，烧结体内部的空隙少。由此可以认为，实施例3的试样中，烧结体与试验片密合，表现出良好的剪切强度。
另一方面，根据图8A和8B可知，比较例3的试样，仅由直径小的银粉(1)和(3)构成，不含直径大的银粉(2-1)或(2-2)，因此银颗粒彼此接触的面积小，未充分融合，因此烧结体内部的空隙多。由此可以认为，比较例3的试样，与实施例3的试样相比，剪切强度变低。
应予说明，根据图7A和7B与图8A和8B的比较可知，比较例3的试样，与实施例3的试样相比，烧结体的部分的厚度变小。针对其原因可以认为，使用芯片安装器将试验片(2)搭载在导电性糊料上时，因芯片安装器的喷嘴载重，导致不含直径大的银粉(2-1)或(2-2)的比较例3将导电性糊料压塌，厚度变小。此外可以认为，比较例3不含直径大的银粉(2-1)或(2-2)，包含更多的溶剂，因此溶剂烧结时蒸发而收缩。
以上，根据表1和2的结果可知，通过使用包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份的导电性糊料，制成烧结体时的导电性优异，此外表现出良好的接合性。

Claims (6)

1.导电性糊料，其特征在于，包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉和溶剂，
相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为15~70质量份，前述具有25μm以上的中位直径D50的银粉的含量为30~85质量份。
2.导电性糊料，其特征在于，包含具有15μm以下的中位直径D50的薄片状银粉、具有25μm以上的中位直径D50的银粉、具有在0.1μm~0.5μm与1μm~15μm具有峰的双峰性的粒度分布的银粉和溶剂，
相对于前述薄片状银粉、前述具有25μm以上的中位直径D50的银粉、和前述具有双峰性的粒度分布的银粉的总计100质量份，前述薄片状银粉的含量为8~55质量份，前述具有25μm以上的中位直径D50的银粉的含量为15~65质量份，前述具有双峰性的粒度分布的银粉的含量为4~45质量份。
3.根据权利要求1所述的导电性糊料，其特征在于，相对于前述薄片状银粉与前述具有25μm以上的中位直径D50的银粉的总计100质量份，前述薄片状银粉的含量为30~42质量份，前述具有25μm以上的中位直径D50的银粉的含量为58~70质量份。
4.根据权利要求2所述的导电性糊料，其特征在于，相对于前述薄片状银粉、前述具有25μm以上的中位直径D50的银粉、和前述具有双峰性的粒度分布的银粉的总计100质量份，前述薄片状银粉的含量为23~35质量份，前述具有25μm以上的中位直径D50的银粉的含量为40~63质量份，前述具有双峰性的粒度分布的银粉的含量为12~35质量份。
5.烧结体，其是将权利要求1~4中任一项所述的导电性糊料烧结而得到的。
6.烧结体，其是将包含基板、权利要求1~4中任一项所述的导电性糊料和导电体的层叠体烧结而得到的。
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