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CN110312810A - 烧结材料、连接结构体、复合粒子、接合用组合物以及烧结材料的制造方法 - Google Patents

烧结材料、连接结构体、复合粒子、接合用组合物以及烧结材料的制造方法 Download PDF

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Publication number
CN110312810A
CN110312810A CN201880012824.7A CN201880012824A CN110312810A CN 110312810 A CN110312810 A CN 110312810A CN 201880012824 A CN201880012824 A CN 201880012824A CN 110312810 A CN110312810 A CN 110312810A
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CN
China
Prior art keywords
agglomerated material
particle
base portion
filling part
kurtosis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201880012824.7A
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English (en)
Inventor
野本博之
笹平昌男
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sekisui Chemical Co Ltd
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Sekisui Chemical Co Ltd
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Filing date
Publication date
Application filed by Sekisui Chemical Co Ltd filed Critical Sekisui Chemical Co Ltd
Priority to CN202210825060.1A priority Critical patent/CN115319082A/zh
Publication of CN110312810A publication Critical patent/CN110312810A/zh
Pending legal-status Critical Current

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    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/05—Mixtures of metal powder with non-metallic powder
    • C22C1/058—Mixtures of metal powder with non-metallic powder by reaction sintering (i.e. gasless reaction starting from a mixture of solid metal compounds)
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    • B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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    • B22F7/06—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
    • B22F7/062—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
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Abstract

本发明提供一种热应力和接合强度均优异的烧结材料、具有该烧结材料的连接结构体、能够制造烧结材料的接合用组合物以及烧结材料的制造方法。本发明提供一种烧结材料，其具有基部(1)、缓冲部(2)以及填充部(3)。缓冲部(2)以及填充部(3)分散存在于基部(1)中。基部(1)是金属的烧结体，缓冲部(2)由空孔以及不同于所述烧结体的材料中的至少一种形成，填充部(3)由粒子以及纤维中的至少一种形成。将烧结材料的三维图像中所述缓冲部的体积分布的峰度设为A，将除去填充部后的所述烧结材料的三维图像中缓冲部的体积分布的峰度设为B时，满足A>B。

Description

烧结材料、连接结构体、复合粒子、接合用组合物以及烧结材 料的制造方法
技术领域
本发明涉及烧结材料以及在连接部具有该烧结材料的连接结构体、复合粒子、接合用组合物以及烧结材料的制造方法。
背景技术
众所周知，以往，在作为用于逆变器等的功率半导体装置(功率器件)中的一种的非绝缘型半导体装置(连接结构体)中，为了固定半导体元件，使用连接部件。该连接部件例如可由固化性的粘接剂或烧结性材料等形成，根据粘接部件的材料种类，也可成为半导体装置的电极之一。
例如，专利文献1、2公开了，利用调整了空孔率的烧结材料作为用于固定半导体元件的连接部件。通过将该烧结材料用作半导体元件的连接部件，而可确保散热性以及接合强度。
现有技术文献
专利文献
专利文献1：日本特开2011-77225号公报
专利文献2：日本特开2014-96545号公报
发明内容
本发明所解决的技术问题
但是，在使用对比文件1、2等所公开的具有空孔的烧结材料作为连接部件的情况下，空孔具有缓和热应力的作用，但也成为强度降低的主要原因。因此，例如，如专利文献2所公开的(第[0012]段)，有此外设置空孔率低的致密层的必要，因此，得到连接部件的工序变得复杂，此外，由于存在空孔率低的致密层，因此存在造成缓和热应力的作用降低的问题。由此，在作为现有的连接部件的烧结材料中，难以兼具缓和热应力的作用以及接合强度，在需要高输出特性的半导体装置的使用中，依然存在改善的余地。
本发明是鉴于上述情况而完成的，本发明的目的在于，提供兼具优异的缓和热应力的作用以及接合强度的烧结材料、具备该烧结材料的连接结构体、复合粒子、用于制造烧结材料的接合用组合物以及烧结材料的制造方法。
解决技术问题的技术手段
本发明人为达成上述目的而进行了深入研究，结果发现，通过控制烧结材料中具有应力缓和作用的缓和部(空孔等)的分布状态，可以达成上述目的，从而完成了本发明。
即，本发明例如包含以下项所记载的发明。
项1、一种烧结材料，其具有基部、缓冲部以及填充部，其中，
所述基部为金属的烧结体，
所述缓冲部以及填充部分散存在于所述基部中，
所述缓冲部由空孔以及不同于所述烧结体的材料中的至少一种形成，
所述填充部由粒子以及纤维中的至少一种形成，
将所述烧结材料的三维图像中所述基部的体积分布的峰度设为A，将除去所述填充部后的所述烧结材料的三维图像中基部的体积分布的峰度设为B时，满足A>B。
项2、一种烧结材料，其具有基部、缓冲部以及填充部，其中，
所述基部为金属的烧结体，
所述缓冲部以及填充部分散存在于所述基部中，
所述缓冲部由空孔以及不同于所述烧结体的材料中的至少一种形成，
所述填充部由粒子以及纤维中的至少一种形成，
将所述烧结材料的三维图像中所述基部的体积分布的峰度设为A时，A的值为0.2以上。
项3、根据项1所述的烧结材料，其中，A-B的值为0.1以上。
项4、根据项1～3中任一项所述的烧结材料，其中，所述填充部的含量为0.01重量％以上且10重量％以下。
项5、根据项1～4中任一项所述的烧结材料，其中，所述填充部之间的最近距离为1μm以上且10μm以下。
项6、根据项1～5中任一项所述的烧结材料，其中，所述基部以在一维方向上具有取向性的形式分布并存在。
项7、一种连接结构体，其在连接部具有项1～6中任一项所述的烧结材料。
项8、一种复合粒子，其用于形成项1～7中任一项所述的烧结材料的填充部，所述复合粒子具有在基材粒子上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材粒子被金属部包覆而成的结构。
项9、一种接合用组合物，其含有复合体和金属粒子，所述复合体具有在基材上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材被金属部包覆而成的结构，其中，将所述接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为A，将除去所述复合体后的接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为B时，满足A>B。
项10、一种接合用组合物，其含有复合体和金属粒子，所述复合体具有在基材上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材被金属部包覆而成的结构，其中，将所述接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为A时，A的值为0.2以上。
项11、一种烧结材料的制造方法，其包含对项9或10所述的接合用组合物进行烧结的工序。
发明效果
根据本发明的烧结材料，其兼具优异的缓和热应力的作用以及接合强度。因此，本发明的烧结材料，例如适用作用于接合半导体元件的接合部件。
本发明的复合粒子，可适用作用于得到所述烧结材料的原料，特别适用作用于形成所述烧结材料的填充部的原料。
附图说明
图1是表示本发明的烧结材料的实施方式的一个实例并且表示其截面的示意图。
图2(a)是说明实施例1中得到的三维图像的图，图2(b)是说明将烧结材料划分为125个区块中的一个区块的图。
图3是用于测定热应力的缓和作用以及接合强度的测定装置的示意图。
具体实施方式
以下，对本发明的实施方式进行详细说明。
图1是表示本发明的烧结材料的截面的示意图。需要说明的是，在本发明中，烧结材料是指通过烧结形成的生成物。
本实施方式的烧结材料具备基部1、缓冲部2以及填充部3。如图1所示，缓冲部2以及填充部3分散存在于基部1中。需要说明的是，虽仅为明确起见的注释，但也可表达为缓冲部2以及填充部3分散存在于烧结材料中。
基部1是金属的烧结体，是成为烧结材料的母体的部分。
缓冲部2由空孔以及不同于所述烧结体的材料中的至少一种形成。一般而言，烧结材料具有空孔，但本发明的烧结材料既存在具有空孔的情况，也存在该空孔的一部分或全部被不同于所述烧结体的材料填充的情况。烧结材料中存在的缓冲部2可仅由空孔形成。或者，烧结材料中存在的缓冲部2可仅由不同于所述烧结体的材料形成。此外，烧结材料也可具有由空孔形成的缓冲部2以及由不同于所述烧结体的材料形成的缓冲部2这两者。
缓冲部2在烧结材料中形成多个，多个缓冲部2可互不凝聚而独立存在。或者，多个缓冲部2的一部分或全部也可在烧结材料中相连(连通)存在。
填充部3由粒子以及纤维中的至少一种形成。填充部3在烧结材料中形成多个。也可存在多个填充部3中的一部分由粒子形成而剩余部分由纤维形成的情况。
多个填充部3可互不凝聚而独立散布于烧结材料中，也可一部分凝聚并存在。就缓冲部2容易分散并存在的观点而言，填充部3优选不凝聚而均匀分散并存在于烧结材料中。
填充部3以其表面的一部分或整体与基部1(烧结体)接触的方式存在。填充部3与基部1的烧结体例如可进行化学键合而接触。该化学键合的种类并无限定。例如，当形成填充部3的粒子和/或纤维如下所述在填充部3的表面具有金属时，所述化学键合可为金属键合。在该情况下，该金属也可与构成基部1的金属形成固溶体。由此，填充部3变得易于不凝聚并均匀分散存在于烧结材料中。
本发明的烧结材料可具有如图1所示的结构。特别是，本发明的烧结材料可分为下述两种形态。以下，将两种形态的烧结材料分别称为第一实施方式、第二实施方式。
第一实施方式的烧结材料中，当将该烧结材料的三维图像中所述基部1的体积分布的峰度设为A，将除去所述填充部3后的所述烧结材料的三维图像中基部1的体积分布的峰度设为B时，满足A>B。
第二实施方式的烧结材料中，当将该烧结材料的三维图像中所述基部1的体积分布的峰度设为A时，A的值为0.2以上。
烧结材料的三维图像可通过对烧结材料的截面进行扫描式电子显微镜(SEM)观察，并利用市售的三维图像解析软件对其进行解析而得到。当进行烧结材料的截面观察时，将烧结材料于多个部位切断，并利用扫描式电子显微镜(SEM)观察各截面。就该切断而言，形成微小的间隔，详细而言根据烧结材料的缓冲部2或填充部3的大小适当设定。所述间隔越小，越可得到准确的三维图像。优选的所述间隔为400nm以下，进一步优选为200nm以下。作为得到三维图像的具体方法，可通过使用了FEI制的“Helios660”的FIB-SEM法，如上所述进行烧结材料的各截面的拍摄，对于所得到的SEM图像，利用所述软件重建三维图像，由此得到三维图像。三维图像的重建例如可使用FEI公司制造的“AVIZO”等软件进行。
可基于所得到的三维图像，以下述顺序测量基部1的体积分布的峰度A(以下，简称为“峰度A”)。
首先，将以上述方式得到的烧结材料的三维图像进一步均等地分割为125个(划分为125个区块)。例如，若烧结材料为立方体，则将该立方体进一步划分为125个立方体(参照下述图2(b))。对于以此方式得到的各区块，观察基部1、缓冲部2以及填充部3，测量各自的体积。该体积的测量例如可使用FEI公司制造的“AVIZO”进行。
基于所述125个区块各自的基部1的体积，制成体积分布，根据该体积分布计算出峰度A。体积分布以及峰度A可使用市售的计算软件例如Microsoft公司制造的“Excel2013”算出。
通过上述方式，可测量烧结材料的三维图像中基部1的体积分布的峰度(峰度A)。
根据日本工业标准(JIS)，峰度作为“尖削度(kurtosis)”，被定义为，平均值附近的四阶中心距μ4与标准偏差σ的四次幂之比μ4/σ4。峰度是表示概率变量的概率密度函数或频率分布的尖锐度的指标。若峰度较大，则与正态分布相比成为具有锐峰以及长粗下摆的分布，若峰度较小，则与正态分布相比成为具有更圆峰以及短细尾的分布。
基部1、缓冲部2以及填充部3分别由不同成分形成，因此在烧结材料的三维图像中，基部1、缓冲部2以及填充部3分别以不同的对比度映出。由此，通过预先确认构成基部1、缓冲部2以及填充部3的成分在三维图像中为哪种对比度，可以容易地判别三维图像中基部1、缓冲部2以及填充部3。
除去填充部3后的所述烧结材料的三维图像中基部1的体积分布的峰度B(以下，简称为“峰度B”)也可基于三维图像进行测量。
此处，“除去填充部3后的烧结材料”是指在用于测量峰度A的烧结材料中仅除掉填充部3后的烧结材料。因此，除不存在填充部3的情况以外，用于测量峰度A的烧结材料与用于测量峰度B的烧结材料相同。
峰度B也可以与测量峰度A的情况相同的顺序进行测量。即，可以得到烧结材料的三维图像，将该三维图像划分为125个区块，根据各区块的基部1的体积分布测量基部1的峰度B。
本发明的烧结材料中，峰度A大于峰度B。该情况表明，具备填充部3的烧结材料相比于不具备填充部3的烧结材料而言基部1的体积分布更均匀。即，相比于不具备填充部3的烧结材料，具备填充部3的烧结材料的基部1的体积分布更均匀，并且可以说缓冲部2的尺寸单分散化。
以往，在掌握烧结材料的特性时，完全未着眼于作为基部1的烧结体的体积分布以及以空孔等缺陷为代表的缓冲部2的分布。然而，本申请的发明人着眼于它们的体积分布，发现若它们更均匀地形成，则烧结材料的热应力的缓和作用以及接合强度这两者均优异。
此外，本发明人发现，通过使基部与填充部具有化学键合，容易产生对热应力的缓和作用。
需要说明的是，在本说明书中，烧结材料的接合强度是指，在以使半导体元件等对象部件接合的目的使用烧结材料的情况下，烧结材料与接合部件之间的接合强度。
在本发明中，可认为分散存在于烧结体(基部1)中且由特定材料形成的填充部3使得缓冲部2以均匀的体积分布分散化。即，可认为填充部3具有能够调节缓冲部2的分布的作用。
第一实施方式的烧结材料中，峰度A与峰度B的差(A-B的值)优选为0.1以上，特别是0.2以上。在该情况下，烧结材料的热应力的缓和作用以及接合强度这两者更优异。
第二实施方式的烧结材料中，峰度A的值为0.2以上，优选为0.3以上，更优选为0.4以上，特别优选为0.5以上。在该情况下，烧结材料的热应力的缓和作用以及接合强度这两者更优异。峰度A的值的上限越大越好，通常为125。
本发明的烧结材料中，填充部3的含量相对于烧结材料的总重量优选为0.01重量％以上且10重量％以下。在该情况下，容易增大峰度A，烧结材料的热应力的缓和作用以及接合强度这两者更优异。填充部3的含量相对于烧结材料的总重量更优选为5重量％以下。
在本发明的烧结材料中，填充部3之间的最近距离优选为1μm以上且10μm以下。在该情况下，可进一步增大峰度A的值，从而使烧结材料的热应力的缓和作用以及接合强度这两者更进一步优异。
填充部3之间的最近距离以如下方式进行测量：从通过与上述相同的方法得到的三维图像中选择50组相邻的一对填充部3，分别测定各组的最表层间的距离，从中以距离较短的顺序选择10组，对该10组的距离进行平均。一对填充部3的最表层之间的距离的测定，例如可使用FEI制的“AVIZO”。
在本发明的烧结材料中，优选为基部1以在一维方向具有取向性的形式分布并存在。在该情况下，具有如下优点：烧结材料的热应力的缓和作用以及接合强度这两者更优异，并且相对于该一维方向垂直的方向的热应力的缓和作用以及接合强度也容易提高。所谓相对于一维方向垂直的方向，例如指相对于烧结材料的表面上的一方向，在该面上垂直的方向。
形成基部1的金属的烧结体的种类并无特别限定。形成烧结体的金属可以与用于形成烧结体的公知的金属相同。例如，作为金属，可举出选自金、银、锡、铜、锗、铟、钯、碲、铊、铋、锌、砷、硒以及含有这些金属元素中的至少1种金属元素的合金中的1种以上。这些之中，优选含有选自金、银以及铜中的1种以上，在该情况下，缓冲部2更易于均匀地分散。
在缓冲部2由不同于烧结体的材料形成的情况下，其材料的种类并无特别限定。例如，形成缓冲部2的材料可举出金属、树脂、有机物、无机物、玻璃、陶瓷等。在缓冲部2为金属的情况下，是指与构成烧结体的金属不同种类的金属元素。作为缓冲部2，优选为树脂、有机物(除树脂以外)、无机物、玻璃、陶瓷等。
就烧结材料的制造较为容易且可以使烧结材料轻量化的观点而言，缓冲部2优选为空孔。
在填充部3由粒子形成的情况下，粒子的种类并无特别限定。作为粒子，可举出树脂粒子、除金属粒子以外的无机粒子、有机无机混合粒子以及金属粒子等。
填充部3特别优选为具有在基材上设置胶体催化剂或烧结促进剂而成的结构的复合体、或者具有基材被金属部包覆而成的结构的复合体。此外，基材优选为粒子，在该情况下，复合体可称为“复合粒子”。此外，将基材为粒子的情形记载为“基材粒子”。
在填充部3由所述复合体形成的情况下，通过复合体的表面存在的胶体催化剂、烧结促进剂或金属部，提高填充部3与作为烧结体的基部1的亲和性，特别是容易产生填充部3与作为烧结体的基部1的化学键合。由此，使填充部3更容易均匀地分散于烧结材料中。其结果，缓冲部2也容易在烧结材料中均匀地分散(单分散化)，峰度A变得更大，特别可提高烧结材料的热应力的缓和作用以及接合强度这两者。此外，由于填充部3与基部1的亲和性提高，因此填充部3的与基部1的接触面积变大。其结果，不易于填充部3与基部1之间产生空隙，特别可提高烧结材料的热应力的缓和作用以及接合强度这两者。复合体特别优选为复合粒子。
基材可举出树脂、除金属以外的无机物、有机无机混合树脂等。在基材为所述基材粒子的情况下，例如可举出树脂粒子、除金属粒子以外的无机粒子、有机无机混合粒子以及金属粒子等。基材粒子优选为树脂粒子、除金属粒子以外的无机粒子或有机无机混合粒子。
在基材或基材粒子为树脂的情况下，可优选使用各种有机物。作为这样的材料，例如可举出：聚乙烯、聚丙烯、聚苯乙烯、聚硅氧烷树脂、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、聚砜、聚碳酸酯、聚酰胺、酚醛树脂(Phenolformaldehyde)、三聚氰胺甲醛树脂、苯并胍胺甲醛树脂、尿素甲醛树脂、酚树脂、三聚氰胺树脂、苯并胍胺树脂、环氧树脂、饱和聚酯树脂、不饱和聚酯树脂、聚苯醚、聚缩醛、聚酰亚胺、聚酰胺酰亚胺、聚醚醚酮以及聚醚砜、尿素树脂等。
在基材为树脂粒子的情况下，也可通过使1种或2种以上的具有烯键式不饱和基的各种聚合性单体聚合而得到。在该情况下，可以设计并合成具有任意物性的树脂粒子。此外，在该情况下，可容易将基材粒子的硬度控制在适宜的范围。就该观点而言，所述树脂粒子的材料优选为使1种或2种以上的具有多个烯键式不饱和基的聚合性单体聚合而成的聚合物。
在使具有烯键式不饱和基的单体聚合而得到所述树脂粒子的情况下，作为该具有烯键式不饱和基的单体，可举出非交联性的单体和/或交联性的单体。需要说明的是，在以下的说明中，“(甲基)丙烯酸”指“丙烯酸”以及“甲基丙烯酸”中的一者或两者，“(甲基)丙烯酸酯”指“丙烯酸酯”以及“甲基丙烯酸酯”中的一者或两者。
作为所述非交联性的单体，例如，作为乙烯化合物，可举出：苯乙烯、α-甲基苯乙烯、氯苯乙烯等苯乙烯类单体；甲基乙烯醚、乙基乙烯醚、丙基乙烯醚、1,4-丁二醇二乙烯醚、环己烷二甲醇二乙烯醚、二乙二醇二乙烯醚等乙烯醚类；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；氯乙烯、氟乙烯等含卤单体；作为(甲基)丙烯酸化合物，可举出：(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-羟基乙酯、(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氧原子的(甲基)丙烯酸酯类；(甲基)丙烯腈等含腈单体；(甲基)丙烯酸三氟甲酯、(甲基)丙烯酸五氟乙酯等含卤(甲基)丙烯酸酯类；作为α-烯烃化合物，可举出：二异丁烯、异丁烯、LINEALENE、乙烯、丙烯等烯烃类；作为共轭二烯化合物，可举出：异戊二烯、丁二烯等。
作为所述交联性的单体，例如，作为乙烯化合物，可举出：二乙烯苯、1,4-二乙烯氧基丁烷、二乙烯砜等乙烯类单体；作为(甲基)丙烯酸化合物，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；作为烯丙基化合物，可举出：(异)氰尿酸三烯丙酯、偏苯三甲酸三烯丙酯、邻苯二甲酸二烯丙酯、二烯丙基丙烯酰胺、二烯丙醚；作为聚硅氧烷化合物，可举出：四甲氧基硅烷、四乙氧基硅烷、三乙基硅烷、叔丁基二甲基硅烷、甲基三甲氧基硅烷、甲基三乙氧基硅烷、乙基三甲氧基硅烷、乙基三乙氧基硅烷、异丙基三甲氧基硅烷、异丁基三甲氧基硅烷、环己基三甲氧基硅烷、正己基三甲氧基硅烷、正辛基三乙氧基硅烷、正癸基三甲氧基硅烷、苯基三甲氧基硅烷、二甲基二甲氧基硅烷、二甲基二乙氧基硅烷、二异丙基二甲氧基硅烷、三甲氧基甲硅烷基苯乙烯、γ-(甲基)丙烯酰氧基丙基三甲氧基硅烷、1,3-二乙烯基四甲基二硅氧烷、甲基苯基二甲氧基硅烷、二苯基二甲氧基硅烷等硅烷烷氧化物类；乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、二甲氧基甲基乙烯基硅烷、二甲氧基乙基乙烯基硅烷、二乙氧基甲基乙烯基硅烷、二乙氧基乙基乙烯基硅烷、乙基甲基二乙烯基硅烷、甲基乙烯基二甲氧基硅烷、乙基乙烯基二甲氧基硅烷、甲基乙烯基二乙氧基硅烷、乙基乙烯基二乙氧基硅烷、对苯乙烯基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基三甲氧基硅烷、3-甲基丙烯酰氧基丙基甲基二乙氧基硅烷、3-甲基丙烯酰氧基丙基三乙氧基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷等含聚合性双键的硅烷烷氧化物；十甲基环五硅氧烷等环状硅氧烷；单末端改性硅油、两末端硅油、侧链型硅油等改性(反应性)硅油；(甲基)丙烯酸、马来酸、马来酸酐等含羧基的单体等。
交联性以及非交联性单体并不限定于上述例举的单体，也可以是其他聚合性单体，例如公知的聚合性单体。
通过公知的方法使所述具有烯键式不饱和基的聚合性单体聚合，由此可得到所述树脂粒子。作为该方法，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子粒子与自由基聚合引发剂一起使单体膨润而进行聚合的方法(所谓的种子聚合法)等。这些聚合方法的条件并无特别限制，可设为公知的条件。
在所述基材为除金属粒子以外的无机或有机无机混合树脂的情况下，关于作为基材的材料的无机物，可举出二氧化硅以及碳黑等。该无机物优选为非金属。所述二氧化硅并无特别限定，例如可举出：通过使具有2个以上的水解性烷氧基甲硅烷基的硅化合物水解而形成交联聚合物粒子后，根据需要进行煅烧而得到的粒子。作为所述有机无机混合树脂，例如可举出：交联的烷氧基甲硅烷基聚合物以及丙烯酸树脂所形成的有机无机混合粒子等。在基材粒子的情况下，可以是除金属粒子以外的无机粒子或有机无机混合树脂粒子。
作为所述基材的材料的其他实例，可举出包含聚轮烷的树脂。聚轮烷是指，链状高分子穿过环状分子的开口部而形成的结构。聚轮烷的种类并无特别限定，例如可举出公知的聚轮烷。若为基材粒子，则可设为含聚轮烷的粒子。
在构成基材的材料为包含聚轮烷的树脂的情况下，聚轮烷优选为交联体。具体而言，优选为聚轮烷中的环状分子与其他聚轮烷中的环状分子通过高分子链交联而成的结构。若为这样的交联聚轮烷，则基材的柔软性变高，因此容易发挥应力缓和效果，由此，在将烧结材料应用于连接结构体的情况下，容易抑制连接结构体的裂缝以及翘曲的产生。即使是这样的作为交联体的聚轮烷，其种类也并无特别限定，例如可举出公知的交联聚轮烷。
所述聚轮烷例如可通过公知的方法进行制造。例如，通过使具备具有聚合性官能团的环状分子的聚轮烷与聚合性单体形成的混合物进行反应，从而制备具有交联结构的聚轮烷。该反应例如可通过公知的方法进行。
具备具有聚合性官能团的环状分子的聚轮烷的种类并无特别限制。具体实例可举出：由ADVANCED SOFT MATERIALS股份有限公司市售的“SERM(注册商标)SUPER POLYMERSM3405P”、“SERM(注册商标)KEY MIXTURE SM3400C”、“SERM(注册商标)SUPER POLYMERSA3405P”、“SERM(注册商标)SUPER POLYMER SA2405P”、“SERM(注册商标)KEY MIXTURESA3400C”、“SERM(注册商标)KEY MIXTURE SA2400C”、“SERM(注册商标)SUPER POLYMERSA3405P”、“SERM(注册商标)SUPER POLYMER SA2405P”等。
就基材粒子的平均粒径而言，例如从确保烧结材料中的填充部3的优异分散性的观点出发，可设为0.1μm以上且50以下。基材粒子的平均粒径优选为1μm以上，更优选为3μm以上，此外，优选为50μm以下，更优选为10μm以下。
所述基材粒子的平均粒径，在形状为圆球状的情况下，指直径，在为圆球状以外的形状的情况下，指最大径与最小径的平均值。而且，基材粒子的平均粒径指利用扫描式电子显微镜观察基材粒子且利用光标卡尺测定随机选择的50个基材粒子的粒径所得的平均值。需要说明的是，在基材粒子如上所述被其他材料包覆的情况下，其平均粒径也包含其包覆层。
基材粒子的粒径的变异系数(CV值)例如为50％以下。所述变异系数(CV值)由下述式表示。
CV值(％)＝(ρ/Dn)×100
ρ：粒子的粒径的标准偏差
Dn：粒子的粒径的平均值。
就容易使缓冲部2单分散化的观点而言，基材粒子的CV值优选为40％以下，更优选为30％以下。基材粒子的粒径的CV值的下限并无特别限定。CV值可以是0％以上，也可以是5％以上，也可以是7％以上，也可以是10％以上。
基材粒子的硬度例如可以是10N/mm2以上且3000N/mm2以下。就烧结材料的热应力的缓和作用以及接合强度这两者容易提高的观点而言，10％K值优选为100N/mm2以上，更优选为1000N/mm2以上，优选为2500N/mm2以下，特别优选为2000N/mm2以下。
此处所述的10％K值是将基材粒子压缩10％时的压缩弹性模量。可通过如下方式测定。首先，使用微小压缩试验机，利用圆柱(直径50μm、金刚石制)的平滑压头端面，在25℃、历时60秒负荷最大试验负载20mN的条件下，将基材粒子压缩。测定此时的负载值(N)以及压缩位移(mm)。可根据所得到的测定值，通过下述式求出所述压缩弹性模量。
10％K值(N/mm2)＝(3/21/2)·F·S-3/2·R-1/2
F：粒子压缩变形10％时的负载值(N)
S：粒子压缩变形10％时的压缩位移(mm)
R：粒子的半径(mm)
微小压缩试验机，使用FISCHER公司制造的“FISCHERSCOPE H-100”等。需要说明的是，在求30％K值的情况下，也可通过求出使粒子压缩变形30％时的所述各参数而算出。
作为所述烧结促进剂或胶体催化剂，可举出金属微粒或助熔剂(flux)成分。
作为所述金属微粒，可举出金、银、铂、钯、锡、铜、锗、铟、钯、锌、铟、锌、铱、铑、钌、锇以及这些的合金等。所述金属微粒可仅为1种，也可包含2种以上。
作为将所述金属微粒配置在基材粒子表面上的方法，例如可举出下述(1)～(3)。
(1)在基材粒子的分散液中添加金属微粒，通过范德瓦尔斯力使所述金属微粒聚集、附着于所述基材粒子的表面的方法。
(2)在放入有基材粒子的容器中添加金属微粒，通过因容器的旋转等产生的机械作用使所述金属微粒附着于所述基材粒子的表面的方法。
(3)在基材粒子的分散液中添加金属纳米胶体，通过化学键合使所述金属纳米胶体聚集于所述基材粒子的表面后，利用还原剂将金属纳米胶体还原并使其金属化，由此使金属微粒附着在基材粒子的表面的方法。
其中，就容易控制附着的金属微粒的量的观点而言，优选为所述(1)的方法。需要说明的是，即使为基材粒子以外的基材，也可采用所述(1)～(3)的方法。
所述金属微粒的平均粒径优选为1nm以上，更优选为5nm以上，优选为1000nm以下，更优选为500nm以下，进一步优选为100nm以下。需要说明的是，在所述金属微粒使用所述(3)的方法中的金属纳米胶体的情况下，优选为1nm以上，更优选为5nm以上，优选为50nm以下，更优选为40nm以下，进一步优选为35nm以下。若所述金属微粒的粒径为所述下限以上以及所述上限以下，则粒子与烧结体的接触面积变大。所述金属纳米胶体的粒径指最大径。所述金属微粒的平均粒径是通过利用穿透式电子显微镜等进行观察并对随机抽选的100个金属微粒的最大径进行平均而求出。
作为所述助熔剂成分，可举出公知的助熔剂，例如可举出树脂类助熔剂、有机类助熔剂、无机类助熔剂等。作为树脂类助熔剂，可举出以松脂酸、长叶松酸(palustric acid)、脱氢松脂酸、异海松酸、新松脂酸、海松酸(pimaric acid)为主成分的松香。作为有机类助熔剂，可举出脂肪族羧酸、芳香族羧酸。作为无机类助熔剂，可举出溴化铵或氯化铵等卤化物。所述助熔剂成分可仅为1种，也可含有2种以上。通过配置在基材粒子的助熔剂成分，在烧结过程中除去烧结体表面上的氧化被膜，在基材粒子表面促进烧结反应，使基材粒子与烧结体的接触面积变大。
在复合体为包覆有金属部的基材的情况下，作为基材的种类，与具有在基材上设置胶体催化剂或烧结促进剂而成的结构的复合体的情形相同。在该情况下，基材也可以是基材粒子。
所述金属部由包含金属的材料形成。作为该金属，例如可举出：金、银、锡、铜、铜、锗、铟、钯、碲、铊、铋、锌、砷、硒、铁、铅、钌、铝、钴、钛、锑、镉、硅、镍、铬、铂、铑等。金属部可仅为这些各金属中的任一种，或者也可包含2种以上。此外，金属部也可以是上述例举的各金属中的2种以上的金属的合金。
金属部例如可以以包覆所述基材的方式形成为层状。在该情况下，金属部可由1层形成，或者也可由多层形成。
金属部的厚度例如可设为0.5nm以上，优选为10nm以上，此外，可设为10μm以下，优选为1μm以下，进一步优选为500nm以下，特别优选为300nm以下。若金属部的厚度为所述下限以上以及所述上限以下，则作为填充部3的复合粒子更容易在基部1中均匀地分散，可使缓冲部2更均匀地分散。
在基材粒子的表面上形成金属部的方法并无特别限定。作为形成金属部的方法，例如可举出利用无电解镀敷的方法、利用电解镀敷的方法、利用物理蒸镀的方法、以及将金属粉末或者含有金属粉末以及粘合剂的糊剂涂布于基材粒子的表面的方法等。就金属部的形成较为简单的观点而言，优选为利用无电解镀敷的方法。作为所述利用物理蒸镀的方法，可举出真空蒸镀、离子镀敷以及离子溅镀等方法。
在金属部为多层结构的情况下，也可通过相同的方法形成金属部。例如，可通过采用所述金属部的形成方法在基材表面形成第一层金属部，在该第一层表面进一步按顺序形成下一层，由此形成多层结构的金属部。
所述金属部也可于外表面具有多个突起。突起例如可通过公知的方法形成。突起的形状以及大小并无特别限定。例如，突起的截面可以是球状或椭圆形状，也可形成为越朝向突起前端越尖的针状。
突起的平均高度可设为1nm以上且1000nm以下，优选为5nm以上，更优选为50nm以上，优选为900nm以下，更优选为500nm以下。若所述突起的平均高度为所述下限以上以及所述上限以下，则复合体(例如，复合粒子)容易与作为烧结体的基部1接触。
突起的平均高度例如可以如下方式测定。以使复合体(例如，复合粒子)的含量成为30重量％的方式添加至KULZER公司制造的“TECHNOVIT4000”，并使之分散，制备复合体检查用嵌入树脂。以通过该检查用嵌入树脂中的分散的复合体的中心附近的方式使用离子研磨装置(HITACHI HIGH-TECHNOLOGIES公司制造的“IM4000”)，切出复合体的截面。然后，使用场发射型扫描式电子显微镜(FE-SEM)，设定为图像倍率5万倍，随机选择20个复合体，观察各复合体的50个突起。将自突起的底面至突起的顶部的高度设为突起的高度，进行算术平均并设为所述突起的平均高度。
突起底面的平均径可设为3nm以上且5000nm以下，优选为50nm以上，更优选为80nm以上，优选为1000nm以下，更优选为500nm以下。此处所谓的突起底面的平均径是指，以与所述突起的平均高度的测定方法相同的顺序，通过使用嵌入树脂的FE-SEM观察，分别观察随机选择的20个复合粒子的突起，测量各基部的两端间距离，对其等进行算术平均而求出的值。
复合体具有在所述基材的表面的一部分或全部配置胶体催化剂或烧结促进剂而成的结构。或者，复合体具有在所述基材的表面的一部分或全部包覆金属部而成的结构。在复合体为复合粒子的情况下，具有在基材粒子的表面的一部分或全部配置胶体催化剂或烧结促进剂而成的结构。或者，复合粒子具有在所述基材的表面的一部分或全部包覆金属部而成的结构。
作为复合粒子的其他形态，也可具备具有凹部的基材粒子以及配置在基材粒子的表面上的胶体催化剂或金属部。在该形态的复合粒子中，也可在凹部包覆胶体催化剂或金属部。
制备具有凹部的基材粒子的方法并无特别限定。例如，可通过对基材粒子进行后处理，在基材粒子形成凹部。利用后处理的凹部的形成方法并无特别限定，例如，可采用公知的方法。具体而言，可举出：对基材粒子的表面进行蚀刻处理的方法、在氧气氛围下进行等离子处理、臭氧处理以及加热处理的方法、进行加湿处理的方法、在真空中进行热处理的方法、在加压以及加湿条件下进行热处理的方法、利用氧化剂进行湿式处理的方法、利用球磨机等进行物理处理的方法等。
凹部的平均深度并无特别限定。例如，凹部的平均深度可设为基材粒子的平均半径的0.1％以上且80％以下。需要说明的是，此处所谓的凹部的深度表示，将具有凹部的基材粒子当作球状时从该球状的基材粒子的表面至成为凹部的最底面的点的距离。具体而言，是指以与所述突起的平均高度的测定方法相同的顺序，通过使用嵌入树脂的FE-SEM观察，分别观察随机选择的20个复合粒子的突起，对各凹部的深度进行算术平均而求出的值。
在复合粒子具有凹部的情况下，复合粒子容易对变形进行追随，其结果，烧结材料的热应力的缓和作用以及接合强度进一步提高。
用于形成填充部3的粒子的形状并无特别限定。作为粒子的形状，例如可举出：球状、椭圆状、不定形状、针状、棒状、板状、鳞片状等。就使填充部3容易均匀地分散于基部1的方面而言，作为粒子的形状，优选为球状或椭圆状。此外，如上所述，就基部1容易以在特定的一维方向具有取向性的形式分布并存在的观点而言，粒子的形状优选为针状、棒状、板状。
就形成填充部3的粒子的平均粒径而言，例如从确保作为烧结体的基部1中的填充部3的分散性的观点出发，可设为0.1μm以上且50μm以下。粒子的平均粒径优选为1μm以上，更优选为3μm以上，此外，优选为10μm以下。
在填充部3由纤维形成的情况下，纤维的种类并无特别限定。作为纤维，例如除天然纤维、合成纤维以外，还可举出玻璃纤维、碳纤维、岩石纤维。天然纤维可举出纤维素、绢、棉、羊毛、麻。合成纤维可举出聚对苯二甲酸乙二醇酯等聚酯、聚酰胺、聚酰亚胺、丙烯酸、聚烯烃、聚甲基戊烯、聚芳酯、聚缩醛、聚苯醚、聚砜、聚醚醚酮、聚苯硫醚。
制造具有所述结构的烧结材料的方法并无特别限制。例如，可通过公知的方法制造烧结材料。
例如，可通过以含有用于形成基部1的金属、用于形成缓冲部2的材料、以及用于形成填充部3的粒子和/或纤维的接合用组合物作为烧结用原料，并将该接合用组合物进行烧结，得到烧结材料。需要说明的是，在得到缓冲部2仅由空孔形成的烧结材料的情况下，接合用组合物不含第二原料。以下，将用于形成基部1的金属称为“第一原料”，将用于形成缓冲部2的材料称为“第二原料”，将用于形成填充部3的粒子和/或纤维称为“第三原料”。
第一原料只要为可形成基部1的烧结体的金属原料，就无特别限制。例如，第一原料可设为金属粒子。金属粒子可以是金属单质粒子，也可以是金属化合物的粒子。金属化合物是含有金属原子以及该金属原子以外的原子的化合物。
作为金属化合物的具体实例，可举出金属氧化物、金属的碳酸盐、金属的羧酸盐以及金属的络合物等。金属化合物优选为金属氧化物。例如，所述金属氧化物是在还原剂的存在下通过连接时的加热成为金属粒子后进行烧结。所述金属氧化物为金属粒子的前体。作为金属的羧酸盐粒子，可举出金属的乙酸盐粒子等。
第一原料的金属可举出选自金、银、锡、铜、锗、铟、钯、碲、铊、铋、锌、砷、硒以及含有这些金属元素中至少1种金属元素的合金中的1种以上。
在第一原料为粒子形状的情况下，其平均粒径可设为10nm以上且10μm以下。此外，第一原料也可含有平均粒径不同的2种以上，在该情况下，可使烧结材料的接合强度提高。例如，平均粒径较小的金属粒子的平均粒径可设为10nm以上且100nm以下，平均粒径较大的金属粒子的平均粒径可设为1μm以上且10μm以下。平均粒径较大的第一原料相对于平均粒径较小的第一原料的混合量之比可设为1/9以上且9以下。需要说明的是，所述平均粒径通过利用扫描式电子显微镜观察金属粒子，对所观察的图像中任意选择的50个各粒子的最大径进行算术平均而求出。
在第一原料为金属氧化物的粒子的情况下，也可组合使用还原剂。作为还原剂，可使用公知的还原剂。还原剂的含量相对于第一原料100重量份，优选为1重量份以上，更优选为10重量份以上，优选为1000重量份以下，更优选为500重量份以下，进一步优选为100重量份以下。若所述还原剂的含量为所述下限以上，则容易得到致密的烧结体。
第一原料中也可根据需要包含其他成分。作为其他成分，例如可举出热塑性树脂或固化性树脂。作为固化性树脂，例如可举出公知的光固化性树脂以及热固化性树脂。光固化性树脂也可含有光固化性树脂以及光聚合引发剂。热固化性树脂也可含有公知的热固化性树脂以及热固化剂。
第一原料中也可含有分散介质。作为分散介质，例如可举出公知的溶剂等。
第一原料也可使用市售的制品。作为具体实例，可举出：KYOCERA CHEMICAL公司制造的“CT2700”、HERAEUS公司制造的“ASP295”、“ASP016”、“ASP043”、HENKEL公司制造的“LOCTITE ABLESTIK SSP2020”、NAMICS公司制造的“H9890-6A”、HARIMA CHEMICALS公司制造的“NH-4000”、“NH-225D”、“NH-3000D”、KAKEN-TECH公司制造的“CM-3212”、“CR-3520”、NIHON SUPERIOR公司制造的“ALCONANO Ag PASTE ANP-1”等。
第一原料优选为具有通过小于400℃的加热进行烧结的性质，更优选为350℃以下，优选为300℃以上。若第一原料的烧结的温度为所述上限以下或小于所述上限，则可有效率地进行烧结，可进一步减少烧结所需的能量且减小环境负荷。
第一原料可仅使用1种，或者也可组合使用2种以上而使用。
在缓冲部2非空孔的情况下，使用第二原料。第二原料可使用不同于第一原料的材料。作为第二原料，与用于形成所述缓冲部2的材料相同。在第二原料为金属的情况下，是指与第二原料中所含的金属不同种类的金属元素。
第三原料与用于形成所述填充部3的粒子和/或纤维相同。
第三原料优选含有所述复合体。在该情况下，在所得到的烧结材料中，填充部3与作为烧结体的基部1的亲和性提高，因此填充部3更容易均匀地分散在烧结材料中。其结果，缓冲部2也容易在烧结材料中均匀地分散(单分散化)，峰度A进一步变大，特别可提高烧结材料的热应力的缓和作用以及接合强度这两者。复合体更优选为复合粒子。
第三原料可仅使用1种，或者也可组合使用2种以上而使用。
在接合用组合物(烧结用原料)中，第一原料、第二原料、第三原料的混合比例并无特别限定。例如，在使用接合用组合物形成烧结材料的情况下，优选以使填充部的含量成为0.01重量％以上且10重量％以下的方式调节第一原料、第二原料、第三原料的含量。需要说明的是，只要不阻碍本发明的效果，则接合用组合物可含有其他原料。接合用组合物也可仅由第一原料、第二原料、第三原料构成。
使接合用组合物烧结的方法并无特别限定。烧结温度可设为100℃以上且400℃以下。如下所述，在加压下进行烧结的情况下，烧结温度优选为150℃以上且350℃以下。此外，在不在加压下进行烧结的情况下，烧结温度优选为200℃以上且350℃以下。
烧结时间例如可设为30秒以上且7200秒以下。如下所述，在加压下进行烧结的情况下，烧结时间优选为180秒以上且600秒以下。此外，在不在加压下进行烧结的情况下，烧结时间优选为180秒以上且5400秒以下。需要说明的是，烧结时间根据烧结温度进行调整即可，例如若设为更高温并缩短烧结时间，则生产效率优异。
烧结也可在加压下进行。该情况下的压力可设为0.1～20MPa。
烧结可以在空气氛围下进行，也可以在氮气等非活性气体氛围下进行。
就容易观察所述三维图像的观点而言，优选在金属板上涂布有接合用组合物的状态下进行烧结。作为金属板，例如可举出铜基板。涂布的方法例如为丝网印刷法。烧结时，也可以在经过丝网涂布的接合用组合物的表面进一步载置其他金属板，在夹入有接合用组合物的状态下进行烧结。
在接合用组合物被烧结而形成烧结体(基部1)的过程中，由于存在第三原料(即，成为填充部3的原料)，因此缓冲部2(例如空孔)不易偏在于烧结体中而容易均匀地分散。由此，达成缓冲部2的单分散化，基部1的体积分布也调整为适当的范围，烧结材料的峰度A变大。
如上所述，通过包括将接合用组合物进行烧结的工序的制造方法，可得到烧结材料。对于以此方式制造的烧结材料，可依据所述顺序来测量烧结材料的峰度A。
另一方面，用于测量峰度B的烧结材料即除去填充部3后的烧结材料(以下，有时称为“空白烧结材料”)例如可以如下方式制造。
通过从所述接合用组合物除去第三原料后进行烧结，可得到空白烧结材料。在该情况下，将第一原料、第二原料的种类以及使用量以及烧结条件设为与得到用于测量峰度A的烧结材料的方法相同的条件。需要说明的是，作为第三原料的除去方法，例如可举出：取接合用组合物，利用光学显微镜进行观察，利用玻璃毛细管从其中除去第三原料的方法；或通过离心分离除去第三原料的方法。或者，在所述烧结材料的制造方法中，使用不含第三原料的接合用组合物进行烧结，由此可得到空白烧结材料。在该情况下，也将第一原料、第二原料的种类以及使用量以及烧结条件设为与得到用于测量峰度A的烧结材料的方法相同的条件。
本发明的接合用组合物特别优选含有复合体和金属粒子，所述复合体具有在所述基材上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材被金属部包覆而成的结构。即，在接合用组合物中，优选第一原料含有所述金属粒子，第三原料含有所述复合体。在该情况下，容易达成缓冲部2的单分散化，基部1的体积分布也容易调整为适当的范围，烧结材料的峰度A变大。需要说明的是，第一原料、第三原料以及其混合比例等的优选方式如上所述。
若使本发明的接合用组合物烧结而形成烧结材料，则可满足A>B。或者，该接合用组合物的烧结材料的A的值可成为0.2以上。其结果，烧结材料的热应力的缓和作用以及接合强度这两者变得更优异，例如适宜作为用于将半导体元件接合的接合部件。
为确认接合用组合物的烧结材料可满足A>B或可满足A≥0.2，将接合用组合物在下述条件下进行烧结。
首先，将接合用组合物以成为100μm的厚度的方式丝网涂布于厚度1mm的Cu基板上，使其表面被厚度1mm的Cu基板夹住。将该夹入的接合用组合物在130℃下且于氮气氛围下干燥90秒钟，然后，一面以5MPa进行加压，一面在300℃下加热3分钟。由此得到烧结材料，因此可使用该烧结材料测量A。此外，通过所述方法从接合用组合物除去第三原料(复合体)，制备用于测定B的组合物，可使用该组合物进行与A的测量相同的方法，由此测量B。
本发明的烧结材料的热应力的缓和作用以及接合强度这两者更优异。因此，本发明的烧结用材料可应用于连接结构体的连接部。在连接部具有本发明的烧结用材料的连接结构体的热应力的缓和作用优异，因此成为耐久性优异的结构体。特别是，连接部含有由本发明的烧结用材料形成的接合部件，因此接合强度也优异。
连接结构体的种类并无特别限定。例如，可举出各种半导体装置(功率装置)。连接结构体的结构例如也可设为与公知的相同。
此外，所述复合体作为用于形成烧结材料的添加剂特别有效。其原因在于：具备所述复合体作为填充部3的烧结材料容易在烧结材料中分散，因此容易有助于缓冲部2的均匀分散化(单分散化)。复合体更优选为复合粒子。
因此，所述复合体适宜作为用于形成所述烧结材料的填充部的添加剂(缓冲部分布调节剂)。即，所述复合体(例如，复合粒子)适合用于使基部1以及缓冲部2分布，适合用于制造烧结材料。
此外，使用含有所述第一原料、第二原料以及第三原料的接合用组合物得到烧结材料的方法也适宜作为调节形成于烧结材料的基部1以及缓冲部2的分布状态的方法。
[实施例]
以下，通过实施例更具体地说明本发明，但本发明并不限定于这些实施例的实施方式。
(实施例1)
作为基材粒子，准备粒径为3.0μm的二乙烯苯共聚物树脂粒子(积水化学工业公司制造的“MICROPEARL SP-203”)。
使用超音波分散器使基材粒子A 10重量份分散于含有钯催化剂液5重量％的碱性溶液100重量份中后，通过对溶液进行过滤，从而取出基材粒子A。继而，将基材粒子A添加至二甲胺硼烷1重量％溶液100重量份中，使基材粒子A的表面活化。将表面活化后的基材粒子A充分水洗后，添加至蒸馏水500重量份中，使其分散，由此得到悬浮液(A)。
将悬浮液(A)放入至含硫酸铜20g/L以及乙二胺四乙酸30g/L的溶液中，得到粒子混合液(B)。
此外，作为无电解镀铜液，准备镀铜液(C)，该镀铜液(C)利用氨将含有硫酸铜250g/L、乙二胺四乙酸150g/L、葡萄糖酸钠100g/L以及甲醛50g/L的混合液调整为pH值10.5。
此外，作为无电解镀银液，准备镀银液(D)，该镀银液(D)利用氨水将含有硝酸银30g/L、琥珀酰亚胺100g/L以及甲醛20g/L的混合液调整为pH值8.0。
在调整为55℃的分散状态的粒子混合液(B)中缓慢滴加所述镀铜液(C)，进行无电解镀铜。镀铜液(C)的滴加速度为30mL/分钟，滴加时间为30分钟，进行无电解镀铜。以该方式得到粒子混合液(E)，该粒子混合液(E)含有于树脂粒子的表面具备铜金属部作为第一金属部的粒子。
然后，通过对粒子混合液(E)进行过滤来提取粒子，并进行水洗，由此得到在所述基材粒子A的表面上配置有铜金属部的粒子。将该粒子充分水洗后，添加至蒸馏水500重量份中，使其分散，由此得到粒子混合液(F)。
然后，在调整为60℃的分散状态的粒子混合液(F)中缓慢滴加所述镀银液(D)，进行无电解镀银。镀银液(D)的滴加速度为10mL/分钟，滴加时间为30分钟，进行无电解镀银。然后，通过进行过滤来取出粒子，并进行水洗、干燥，由此得到在基材粒子A的表面上具备依次叠层铜以及银而成的金属部(金属部整体的厚度：0.1μm)的复合粒子A。
将作为第一原料的银糊剂(NIHON SUPERIOR公司制造的“ALCONANO Ag PASTEANP-1”)0.98g以及所述复合粒子A0.02g，通过刮刀进行混练以充分分散，制备接合用组合物。
将混练后的接合用组合物以成为100μm的厚度的方式丝网涂布于厚度1mm的Cu基板上，使其表面被厚度1mm的Cu基板夹入。将夹入的接合用组合物于130℃下且于氮气氛围下干燥90秒钟，然后，一面以5MPa进行加压，一面于300℃下加热3分钟，由此得到烧结材料。烧结材料中，复合粒子的含量为2重量％，复合粒子间的最近距离为3.52μm。
对于所得到的烧结材料，使用FEI制的“HELIOS660”，通过FIB-SEM法进行断层摄影，重建该图像，得到烧结材料的三维图像。作为观察条件，于加速电压2kv下设为反射电子像，将试样倾斜设为52°。
图2(a)表示实施例1中所得到的三维图像，表示整体图像以及三个断层摄影图像(截面图像)。此外，如图2(b)所示，图2(a)的三维图像是将烧结材料划分为125个区块中的一个区块。
如图2(a)所示，所得到的烧结材料显示出3种不同的对比度，确认形成有基部1、缓冲部2以及填充部3。基部1是银糊剂的烧结体(银烧结体)，填充部3是复合粒子。此外，在本实施例中，缓冲部2是空孔。
使用FEI公司制造的“AVIZO”算出所得到的125个区块各自的基部1、缓冲部2、填充部3的体积，制成体积分布，根据该体积分布算出峰度A，结果为0.97。
另一方面，准备从所述实施例1的接合用组合物除去了复合粒子的组成的接合用组合物，作为峰度B测定用的接合用组合物。
将所得到的峰度B测定用的接合用组合物以成为100μm的厚度的方式丝网涂布于厚度1mm的Cu基板上，使其表面被厚度1mm的Cu基板夹入。将该夹入的接合用组合物在130℃下且在氮气氛围下干燥90秒钟，然后，一面以5MPa进行加压，一面在300℃下加热3分钟，由此得到烧结材料。通过与峰度A相同的方法测量该烧结材料的峰度B，结果为0.52。
(热应力的缓和作用以及接合强度的评价)
热应力的缓和作用以及接合强度是基于“JIS Z 3198-7：无铅焊锡试验方法-第7部芯片部件的焊锡接头剪切试验方法”中记载的“焊锡接头剪切试验方法”进行评价。
图3是示意性地表示用于测定热应力的缓和作用以及接合强度的测定装置。在该测定中，使用圆筒状的铜(径10mm且厚5mm)作为基板100。在基板100上涂布各实施例以及比较例中得到的任一种接合用组合物，形成糊剂层(径5mm且厚50μm)。然后，在该糊剂层上配置铜制的圆盘芯片101(径5mm且厚2mm)，一面以5MPa进行加压，一面在300℃下烧结3分钟，由此利用烧结材料将基板100与芯片101接合。将其置于剪切强度试验机105，以剪切速度6mm/分钟，对芯片101以及接合部施加负载，将位移与负载的关系图表化，得到应力-应变曲线，测量热应力的功以及接合强度。热应力的功可通过算出应力-应变曲线中位移开始后至断裂点为止的积分值来进行测量，表示直至断裂为止所吸收的能量。接合强度是应力-应变曲线中断裂点的应力值。
使用实施例1的接合用组合物进行热应力的缓和作用以及接合强度的评价，其结果，热应力的功为0.988J，接合强度为85.04MPa，能够赋予较以往优异的热应力的缓和作用以及接合强度。
(实施例2)
将作为第一原料的银糊剂变更为0.99g，将所述复合粒子A变更为0.01g，除此以外，通过与实施例1相同的方法制备接合用组合物。复合粒子的含量为1重量％。将所得到的接合用组合物通过与实施例1相同的方法制备烧结材料，通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
(实施例3)
将作为第一原料的银糊剂变更为0.90g，将所述复合粒子A变更为0.10g，除此以外，通过与实施例1相同的方法制备接合用组合物。复合粒子的含量为10重量％。将所得到的接合用组合物通过与实施例1相同的方法制备烧结材料，通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
(实施例4)
将作为第一原料的银糊剂变更为KYOCERA CHEMICAL公司制造的放入有树脂的银糊剂“CT2700”0.98g，除此以外，通过与实施例1相同的方法制备接合用组合物。复合粒子的含量为2重量％。将所得到的接合用组合物以成为100μm的厚度的方式丝网涂布于厚度1mm的Cu基板上，使其表面被厚度1mm的Cu基板夹入。通过将该夹入的接合用组合物在200℃下加热90分钟而得到烧结材料。通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
(实施例5)
使用作为纤维的“L-MWNT-4060(NTP公司制造)”0.02g代替复合粒子A，除此以外，通过与实施例1相同的方法制备接合用组合物。纤维的含量为2重量％。将所得到的接合用组合物通过与实施例1相同的方法制备烧结材料，通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
(比较例1)
仅将作为第一原料的银糊剂(NIHON SUPERIOR公司制造的“ALCONANO Ag PASTEANP-1”)作为接合用组合物。将所得到的接合用组合物通过与实施例1相同的方法制备烧结材料，通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
(比较例2)
仅将作为第一原料的银糊剂(KYOCERA CHEMICAL公司制造的“CT2700”)作为接合用组合物。将所得到的接合用组合物通过与实施例1相同的方法制备烧结材料，通过与所述方法相同的方法分别测定该烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度。
表1是使用各实施例以及比较例中得到的接合用组合物制备的烧结材料的峰度A、峰度B、热应力的功、断裂伸长率以及接合强度的评价结果的总结。
[表1]
根据表1可知，在使用了实施例2～5的接合用组合物的情况下，也可赋予较以往优异的热应力的缓和作用以及接合强度(均为45MPa以上)。
在任一实施例中，均可赋予优异的热应力的缓和作用以及接合强度，可以说其原因在于：在满足A>B的基础上，进一步填充部3(复合粒子A或纤维)与基部1(银烧结体)形成有化学键(例如金属键)。
符号说明
1：基部
2：缓冲部
3：填充部

Claims (11)

1.一种烧结材料，其具有基部、缓冲部以及填充部，其中，
所述基部是金属的烧结体，
所述缓冲部以及填充部分散存在于所述基部中，
所述缓冲部由空孔以及不同于所述烧结体的材料中的至少一种形成，
所述填充部由粒子以及纤维中的至少一种形成，
将所述烧结材料的三维图像中所述基部的体积分布的峰度设为A，将除去所述填充部后的所述烧结材料的三维图像中基部的体积分布的峰度设为B时，满足A>B。
2.一种烧结材料，其具有基部、缓冲部以及填充部，其中，
所述基部是金属的烧结体，
所述缓冲部以及填充部分散存在于所述基部中，
所述缓冲部由空孔以及不同于所述烧结体的材料中的至少一种形成，
所述填充部由粒子以及纤维中的至少一种形成，
将所述烧结材料的三维图像中所述基部的体积分布的峰度设为A时，A的值为0.2以上。
3.根据权利要求1所述的烧结材料，其中，
A-B的值为0.1以上。
4.根据权利要求1～3中任一项所述的烧结材料，其中，
所述填充部的含量为0.01重量％以上且10重量％以下。
5.根据权利要求1～4中任一项所述的烧结材料，其中，
所述填充部之间的最近距离为1μm以上且10μm以下。
6.根据权利要求1～5中任一项所述的烧结材料，其中，
所述基部以在一维方向上具有取向性的形式分布并存在。
7.一种连接结构体，其在连接部具有权利要求1～6中任一项所述的烧结材料。
8.一种复合粒子，其用于形成权利要求1～7中任一项所述的烧结材料的填充部，所述复合粒子具有在基材粒子上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材粒子被金属部包覆而成的结构。
9.一种接合用组合物，其含有复合体和金属粒子，所述复合体具有在基材上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材被金属部包覆而成的结构，其中，
将所述接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为A，将除去所述复合体后的接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为B时，满足A>B。
10.一种接合用组合物，其含有复合体和金属粒子，所述复合体具有在基材上设置胶体催化剂或烧结促进剂而成的结构，或者具有基材被金属部包覆而成的结构，其中，
将所述接合用组合物的烧结材料的三维图像中基部的体积分布的峰度设为A时，A的值为0.2以上。
11.一种烧结材料的制造方法，其包括对权利要求9或10所述的接合用组合物进行烧结的工序。
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