TWI765971B - 燒結材料、連接結構體、複合粒子、接合用組成物及燒結材料之製造方法 - Google Patents

燒結材料、連接結構體、複合粒子、接合用組成物及燒結材料之製造方法 Download PDF

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TWI765971B
TWI765971B TW107105793A TW107105793A TWI765971B TW I765971 B TWI765971 B TW I765971B TW 107105793 A TW107105793 A TW 107105793A TW 107105793 A TW107105793 A TW 107105793A TW I765971 B TWI765971 B TW I765971B
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sintered material
base
sintered
particles
metal
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TW107105793A
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TW201839864A (zh
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野本之
笹平昌男
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日商積水化學工業股份有限公司
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    • 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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Abstract

本發明提供一種熱應力及接合強度之兩者優異之燒結材料、具備該燒結材料之連接結構體、可製造燒結材料之接合用組成物及燒結材料之製造方法。
本發明之燒結材料具備基部1、緩衝部2及填充部3。緩衝部2及填充部3分散存在於基部1中。基部1係金屬之燒結體，緩衝部2由孔隙及不同於上述燒結體之材料中至少任一者形成，填充部3由粒子及纖維中至少任一者形成。於將燒結材料之三維影像中之上述基部之體積分佈之峰度設為A，且將經去除填充部之上述燒結材料之三維影像中之基部之體積分佈之峰度設為B時，滿足A>B。

Description

燒結材料、連接結構體、複合粒子、接合用組成物及燒結材料之製造方法
本發明係關於一種燒結材料、及於連接部具有該燒結材料之連接結構體、複合粒子、接合用組成物、以及燒結材料之製造方法。
眾所周知，以往，於作為用於反相器等之功率半導體裝置(功率裝置)之一的非絕緣型半導體裝置(連接結構體)中，為了固定半導體元件，會使用連接構件。此種連接構件例如可由硬化性之接著劑或燒結性材料等形成，且根據接著構件之材料種類，亦可成為半導體裝置之電極之一。
例如，專利文獻1、2揭示有利用經調整孔隙率之燒結材料作為用以固定半導體元件之連接構件之情況。藉由將此種燒結材料用作半導體元件之連接構件，而可確保散熱性及接合強度。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2011-77225號公報
[專利文獻2]日本特開2014-96545號公報
然而，於將專利文獻1、2等中揭示之具有孔隙之燒結材料用作連接構件之情形時，孔隙雖具有緩和熱應力之作用，但另一方面會成為使強度下降之因素。因此，例如，如專利文獻2所揭示般(段落[0012])，必須另外設置氣孔率較低之緻密層，因此獲得連接構件之步驟變得複雜，又，會有如下問題：由於氣孔率較低之緻密層之存在而發生緩和熱應力之作用降低。如此，根據以往之作為連接構件之燒結材料，難以兼顧緩和熱應力之作用及接合強度，對用於要求高輸出特性之半導體裝置而言，依然留有改善之餘地。
本發明係鑒於上述而完成者，目的在於提供一種緩和熱應力之作用及接合強度兩者優異之燒結材料、具備該燒結材料之連接結構體、複合粒子、用以製造燒結材料之接合用組成物及燒結材料之製造方法。
本發明人等為達成上述目的而反覆進行了努力研究，結果發現藉由控制發揮應力緩和作用之緩和部(孔隙等)於燒結材料中之分佈狀態，而可達成上述目的，從而完成了本發明。
即，本發明例如包含以下之項所記載之發明。
項1.一種燒結材料，其具備基部、緩衝部及填充部，上述基部係金屬之燒結體，上述緩衝部及填充部分散存在於上述基部中，上述緩衝部由孔隙及不同於上述燒結體之材料中至少任一者形成，上述填充部由粒子及纖維中至少任一者形成，於將上述燒結材料之三維影像中之上述基部之體積分佈之峰度設為A，且將經去除上述填充部之上述燒結材料之三維影像中之基部之體積分佈之峰度設為B時，滿足A>B。
項2.一種燒結材料，其具備基部、緩衝部及填充部， 上述基部係金屬之燒結體，上述緩衝部及填充部分散存在於上述基部中，上述緩衝部由孔隙及不同於上述燒結體之材料中至少任一者形成，上述填充部由粒子及纖維中至少任一者形成，於將上述燒結材料之三維影像中之上述基部之體積分佈之峰度設為A時，A之值為0.2以上。
項3.如項1記載之燒結材料，其中，A-B之值為0.1以上。
項4.如項1至3中任一項記載之燒結材料，其中，上述填充部之含量為0.01重量%以上且10重量%以下。
項5.如項1至4中任一項記載之燒結材料，其中，上述填充部彼此之最接近距離為1μm以上且10μm以下。
項6.如項1至5中任一項記載之燒結材料，其中，上述基部以於一維方向具有配向性之方式分佈而存在。
項7.一種連接結構體，其於連接部具有項1至6中任一項記載之燒結材料。
項8.一種複合粒子，其係為了形成項1至7中任一項記載之燒結材料的填充部而使用，具有下述之結構：於基材粒子配置有膠體觸媒或燒結促進劑之結構或者於基材粒子被覆有金屬部之結構。
項9.一種接合用組成物，其含有下述之複合體及金屬粒子，該複合體為：具有於基材配置有膠體觸媒或燒結促進劑之結構、或者具有於基材被覆有金屬部之結構，於將上述接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為A，且將經去除上述複合體之接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為B時，滿足A>B。
項10.一種接合用組成物，其含有下述之複合體及金屬粒子，該複合體為： 具有於基材配置有膠體觸媒或燒結促進劑之結構、或者具有於基材被覆有金屬部之結構，於將上述接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為A時，A之值為0.2以上。
項11.一種燒結材料之製造方法，其包括將項9或10記載之接合用組成物進行燒結之步驟。
根據本發明之燒結材料，熱應力之緩和作用及接合強度兩者優異。因此，本發明之燒結材料例如適宜作為用以將半導體元件接合之接合構件。
本發明之複合粒子可適宜用作用以獲得上述燒結材料之原料，尤其適宜作為用於形成上述燒結材料之填充部之原料。
1‧‧‧基部
2‧‧‧緩衝部
3‧‧‧填充部
圖1表示本發明之燒結材料之實施形態之一例，為表示其剖面之示意圖。
圖2中，(a)係說明實施例1中所獲得之三維影像之圖，(b)係說明將燒結材料劃分為125個區塊中之一個區塊之圖。
圖3係用以測定熱應力之緩和作用及接合強度的測定裝置之示意圖。
以下，對本發明之實施形態進行詳細說明。
圖1係表示本發明之燒結材料之剖面的示意圖。再者，於本發明中，所謂燒結材料，係指藉由燒結形成之產物。
本實施形態之燒結材料具備基部1、緩衝部2及填充部3。如圖1所示，緩衝部2及填充部3分散存在於基部1中。再者，雖僅為明確起見之註釋，但亦可表達為緩衝部2及填充部3分散存在於燒結材料中。
基部1係金屬之燒結體，係成為燒結材料之母體之部分。
緩衝部2由孔隙及不同於上述燒結體之材料中至少任一者形成。一般而言，燒結材料具有孔隙，但本發明之燒結材料既有具有孔隙之情況，亦有該孔隙之一部分或全部被不同於上述燒結體之材料填充之情況。燒結材料中存在之緩衝部2可僅由孔隙形成。或者，燒結材料中存在之緩衝部2可僅由不同於上述燒結體之材料形成。又，燒結材料亦可具有由孔隙形成之緩衝部2及由不同於上述燒結體之材料形成之緩衝部2這兩者。
緩衝部2於燒結材料中形成多個，多個緩衝部2可互不凝聚而獨立存在。或者，多個緩衝部2之一部分或全部亦可於燒結材料中相連(連通)而存在。
填充部3由粒子及纖維中至少任一者形成。填充部3於燒結材料中形成多個。亦可存在多個填充部3中之一部分由粒子形成而剩餘部分由纖維形成之態樣。
多個填充部3可互不凝聚而獨立散佈於燒結材料中，亦可一部分凝聚而存在。就緩衝部2容易分散而存在之觀點而言，填充部3較佳為不凝聚而均勻地分散存在於燒結材料中。
填充部3以其表面之一部分或整體與基部1(燒結體)接觸之方式存在。填充部3與基部1之燒結體例如可進行化學鍵結而接觸。此種化學鍵結之種類並無限定。例如，當形成填充部3之粒子及/或纖維為如下述般於填充部3之表面具有金屬時，上述化學鍵結可成為金屬鍵結。於該情形時，該金屬亦可與構成基部1之金屬形成固溶體。藉此，填充部3容易不凝聚而均勻地分散 存在於燒結材料中。
本發明之燒結材料可具有如圖1所示之結構。尤其是，本發明之燒結材料可分為下述兩種形態。以下，將兩種形態之燒結材料分別稱為第1實施形態、第2實施形態。
第1實施形態之燒結材料於將該燒結材料之三維影像中之上述基部1之體積分佈之峰度設為A，且將經去除上述填充部3之上述燒結材料之三維影像中之基部1之體積分佈之峰度設為B時，滿足A>B。
第2實施形態之燒結材料於將該燒結材料之三維影像中之上述基部1之體積分佈之峰度設為A時，A之值為0.2以上。
燒結材料之三維影像可藉由對燒結材料之剖面進行掃描式電子顯微鏡(SEM)觀察並利用市售之三維影像解析軟體對其進行解析而獲得。當進行燒結材料之剖面觀察時，將燒結材料於多個部位切斷，並利用掃描式電子顯微鏡(SEM)觀察各剖面。該切斷形成微細之間隔，詳細而言根據燒結材料之緩衝部2或填充部3之大小適當設定。上述間隔越小，越可獲得準確之三維影像。較佳之上述間隔為400nm以下，進而較佳為200nm以下。作為獲得三維影像之具體方法，可藉由使用FEI製之「Helios660」之FIB-SEM法，如上述般進行燒結材料之各剖面之攝影，並針對所獲得之SEM影像，利用上述軟體重建三維影像，藉此獲得三維影像。三維影像之重建例如可使用FEI公司製造之「AVIZO」等軟體進行。
可基於所獲得之三維影像，依以下順序計測基部1之體積分佈之峰度A(以下，簡記為「峰度A」)。
首先，將以上述方式獲得之燒結材料之三維影像進而均等地分割為125個(劃分為125個區塊)。例如，若燒結材料為立方體，則將該立方體進而劃分為125個立方體(參照下述圖2(b))。針對以此方式獲得之各區塊 之各者，觀察基部1、緩衝部2及填充部3，並計測各自之體積。該體積之計測例如可使用FEI公司製造之「AVIZO」進行。
基於上述125個區塊各自之基部1之體積，製成體積分佈，根據該體積分佈算出峰度A。體積分佈及峰度A可使用市售之計算軟體例如Microsoft公司製造之「Excel2013」而算出。
以上述方式可計測燒結材料之三維影像中之基部1之體積分佈之峰度(峰度A)。
根據日本工業標準(JIS)，峰度係作為「尖度(kurtosis)」，由平均值附近之四次動差μ4與標準偏差σ之四次冪之比μ4/σ4定義。峰度係表示概率變數之概率密度函數或頻率分佈之尖銳度的指標。若峰度較大，則與常態分佈相比成為具有銳峰及長粗下擺之分佈，若峰度較小，則與常態分佈相比成為具有更圓峰及短細尾之分佈。
基部1、緩衝部2及填充部3分別由不同成分形成，因此於燒結材料之三維影像中，基部1、緩衝部2及填充部3之各者以不同之對比度映出。由此，藉由預先確認構成基部1、緩衝部2及填充部3之成分於三維影像中為哪種對比度，而可容易判別三維影像中之基部1、緩衝部2及填充部3。
經去除填充部3之上述燒結材料之三維影像中之基部1之體積分佈之峰度B(以下，簡記為「峰度B」)亦可基於三維影像進行計測。
此處，所謂「經去除填充部3之燒結材料」，係指於用以計測峰度A之燒結材料中僅除掉填充部3之燒結材料。因此，除不存在填充部3之情況以外，用以計測峰度A之燒結材料與用以計測峰度B之燒結材料相同。
峰度B亦可以與計測峰度A之情形相同之順序進行計測。即，可獲得燒結材料之三維影像，將該三維影像劃分為125個區塊，根據各區塊之基部1之體積分佈計測基部1之峰度B。
根據本發明之燒結材料，峰度A大於峰度B。該情況意指具備填充部3之燒結材料相較於不具備填充部3之燒結材料而言基部1之體積分佈更均勻。即，相較於不具備填充部3之燒結材料，具備填充部3之燒結材料之基部1之體積分佈更均勻，而且可以說緩衝部2之大小單分散化。
以往，於掌握燒結材料之特性時，完全未著眼於：作為基部1之燒結體之體積分佈、及以孔隙等缺陷為代表之緩衝部2之分佈。然而，本案發明人等著眼於其等之體積分佈，發現若其等之體積分佈更均勻地形成，則燒結材料之熱應力之緩和作用及接合強度兩者優異。
進而，本發明人等發現藉由使基部與填充部具有化學鍵而容易產生“對熱應力之緩和作用”。
再者，於本說明書中，所謂燒結材料之接合強度，於以使半導體元件等對象構件接合之目的使用燒結材料之情形時，係指燒結材料與接合構件之接著強度。
於本發明中，認為分散存在於燒結體(基部1)中且由特定材料形成之填充部3使緩衝部2以均勻之體積分佈分散化。即，認為填充部3具有可調節緩衝部2之分佈之作用。
根據第1實施形態之燒結材料，峰度A與峰度B之差(A-B之值)較佳為0.1以上，尤其是0.2以上。於該情形時，燒結材料之熱應力之緩和作用及接合強度兩者更優異。
根據第2實施形態之燒結材料，峰度A之值為0.2以上，較佳為0.3以上，更佳為0.4以上，尤佳為0.5以上。於該情形時，燒結材料之熱應力之緩和作用及接合強度兩者更優異。峰度A之值之上限越大越佳，通常為125。
本發明之燒結材料較佳為填充部3之含量相對於燒結材料之總重量為0.01重量%以上且10重量%以下。於該情形時，容易增大峰度A，燒結材料 之熱應力之緩和作用及接合強度兩者更優異。填充部3之含量更佳為相對於燒結材料之總重量為5重量%以下。
於本發明之燒結材料中，填充部3彼此之最接近距離較佳為1μm以上且10μm以下。於該情形時，可進一步增大峰度A之值，從而使燒結材料之熱應力之緩和作用及接合強度兩者進而更優異。
填充部3彼此之最接近距離係以如下方式進行計測：自藉由與上述相同之方法獲得之三維影像選擇50組相鄰之一對填充部3，分別測定各組之最表層間之距離，從中以距離長短之順序選擇10組，對該10組之距離進行平均。一對填充部3之最表層彼此之距離之測定例如可使用FEI製之「AVIZO」。
於本發明之燒結材料中，較佳為基部1以於一維方向具有配向性之方式分佈而存在。於該情形時，具有如下優點：燒結材料之熱應力之緩和作用及接合強度兩者更優異，並且相對於該一維方向呈正交之方向的熱應力之緩和作用及接合強度亦容易提昇。所謂相對於一維方向呈正交之方向，例如指相對於燒結材料之面上之一方向，於該面上正交之方向。
形成基部1之金屬之燒結體之種類並無特別限定。形成燒結體之金屬可設為與用於形成燒結體的公知之金屬相同。例如，作為金屬，可列舉選自由金、銀、錫、銅、鍺、銦、鈀、碲、鉈、鉍、鋅、砷、硒及含有該等金屬元素中之至少1種金屬元素之合金所構成之群中1種以上。該等之中，較佳為含有選自由金、銀及銅所構成之群中1種以上，於該情形時，緩衝部2容易更均勻地分散。
於緩衝部2由不同於燒結體之材料形成之情形時，其材料之種類並無特別限定。例如，形成緩衝部2之材料可列舉金屬、樹脂、有機物、無機物、玻璃、陶瓷等。於緩衝部2為金屬之情形時，係指與構成燒結體之金屬不同種類之金屬元素。作為緩衝部2，較佳為樹脂、有機物(除樹脂以外)、無 機物、玻璃、陶瓷等。
就燒結材料之製造較為容易且可使燒結材料輕量化之觀點而言，緩衝部2較佳為孔隙。
於填充部3由粒子形成之情形時，粒子之種類並無特別限定。作為粒子，可列舉樹脂粒子、除金屬粒子以外之無機粒子、有機無機混合粒子及金屬粒子等。
填充部3尤佳為具有：於基材配置有膠體觸媒或燒結促進劑之結構之複合體、或者具有於基材被覆有金屬部之結構之複合體。進而，基材較佳為粒子，於該情形時，複合體可稱為「複合粒子」。又，將基材為粒子之情形記載為「基材粒子」。
於填充部3由上述複合體形成之情形時，藉由複合體之表面存在之膠體觸媒、燒結促進劑或金屬部，而填充部3與作為燒結體之基部1的親和性提高，尤其是容易產生填充部3與作為燒結體之基部1的化學鍵結。藉此，填充部3容易更均勻地分散於燒結材料中。其結果，緩衝部2亦容易於燒結材料中均勻地分散(單分散化)，峰度A變得更大，尤其可提昇燒結材料之熱應力之緩和作用及接合強度兩者。又，由於填充部3與基部1之親和性提高，因此填充部3之與基部1之接觸面積變大。其結果，不易於填充部3與基部1之間產生空隙，尤其可提昇燒結材料之熱應力之緩和作用及接合強度兩者。複合體尤佳為複合粒子。
基材可例示樹脂、除金屬以外之無機物、有機無機混合樹脂等。於基材為上述基材粒子之情形時，例如可列舉樹脂粒子、除金屬粒子以外之無機粒子、有機無機混合粒子及金屬粒子等。基材粒子較佳為樹脂粒子、除金屬粒子以外之無機粒子或有機無機混合粒子。
於基材或基材粒子為樹脂之情形時，可較佳地使用各種有機 物。作為此種材料，例如可列舉：聚乙烯、聚丙烯、聚苯乙烯、聚矽氧樹脂、聚氯乙烯、聚偏二氯乙烯、聚異丁烯、聚丁二烯等聚烯烴樹脂；聚甲基丙烯酸甲酯、聚丙烯酸甲酯等丙烯酸樹脂；聚對苯二甲酸烷二酯、聚碸、聚碳酸酯、聚醯胺、酚甲醛樹脂(phenolformaldehyde)、三聚氰胺-甲醛樹脂、苯并胍胺-甲醛樹脂、尿素甲醛樹脂、酚樹脂、三聚氰胺樹脂、苯并胍胺樹脂、環氧樹脂、飽和聚酯樹脂、不飽和聚酯樹脂、聚伸苯醚、聚縮醛、聚醯亞胺、聚醯胺醯亞胺、聚醚醚酮、及聚醚碸、尿素樹脂等。
於基材為樹脂粒子之情形時，亦可藉由使1種或2種以上之具有乙烯性不飽和基之各種聚合性單體聚合而獲得。於該情形時，可設計及合成具有任意物性之樹脂粒子。又，於該情形時，可容易將基材粒子之硬度控制於適宜之範圍。就此種觀點而言，上述樹脂粒子之材料較佳為使1種或2種以上之具有多個乙烯性不飽和基之聚合性單體聚合而成之聚合物。
於使具有乙烯性不飽和基之單體聚合而獲得上述樹脂粒子之情形時，作為該具有乙烯性不飽和基之單體，可列舉非交聯性之單體及/或交聯性之單體。再者，於以下之說明中，「(甲基)丙烯酸」係指「丙烯酸」及「甲基丙烯酸」中之一者或兩者，「(甲基)丙烯酸酯」係指「丙烯酸酯」及「甲基丙烯酸酯」中之一者或兩者。
作為上述非交聯性之單體，例如，作為乙烯化合物，可列舉：苯乙烯、α-甲基苯乙烯、氯苯乙烯等苯乙烯系單體；甲基乙烯醚、乙基乙烯醚、丙基乙烯醚、1,4-丁二醇二乙烯醚、環己烷二甲醇二乙烯醚、二乙二醇二乙烯醚等乙烯醚類；乙酸乙烯酯、丁酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯等酸乙烯酯類；氯乙烯、氟乙烯等含鹵單體；作為(甲基)丙烯酸化合物，可列舉：(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸丁酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸鯨蠟 酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸環己酯、(甲基)丙烯酸異莰酯等(甲基)丙烯酸烷基酯類；(甲基)丙烯酸2-羥基乙酯、甘油(甲基)丙烯酸酯、聚氧乙烯(甲基)丙烯酸酯、(甲基)丙烯酸縮水甘油酯等含氧原子之(甲基)丙烯酸酯類；(甲基)丙烯腈等含腈單體；(甲基)丙烯酸三氟甲酯、(甲基)丙烯酸五氟乙酯等含鹵(甲基)丙烯酸酯類；作為α-烯烴化合物，可列舉：二異丁烯、異丁烯、Linealene、乙烯、丙烯等烯烴類；作為共軛二烯化合物，可列舉：異戊二烯、丁二烯等。
作為上述交聯性之單體，例如，作為乙烯化合物，可列舉：二乙烯苯、1,4-二乙烯氧基丁烷、二乙烯碸等乙烯系單體；作為(甲基)丙烯酸化合物，可列舉：四羥甲基甲烷四(甲基)丙烯酸酯、四羥甲基甲烷三(甲基)丙烯酸酯、四羥甲基甲烷二(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、二新戊四醇六(甲基)丙烯酸酯、二新戊四醇五(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)四亞甲基二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯等多官能(甲基)丙烯酸酯類；作為烯丙基化合物，可列舉：(異)氰尿酸三烯丙酯、偏苯三甲酸三烯丙酯(triallyl trimellitate)、鄰苯二甲酸二烯丙酯、二烯丙基丙烯醯胺、二烯丙醚；作為聚矽氧化合物，可列舉：四甲氧基矽烷、四乙氧基矽烷、三乙基矽烷、第三丁基二甲基矽烷、甲基三甲氧基矽烷、甲基三乙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、異丙基三甲氧基矽烷、異丁基三甲氧基矽烷、環己基三甲氧基矽烷、正己基三甲氧基矽烷、正辛基三乙氧基矽烷、正癸基三甲氧基矽烷、苯基三甲氧基矽烷、二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、二異丙基二甲氧基矽烷、三甲氧基矽基苯乙烯、γ-(甲基)丙烯醯氧基丙基三甲氧基矽烷、1,3-二乙烯基四甲基二矽氧烷、甲基苯基二甲氧基矽烷、二苯基二甲氧基矽烷等矽烷烷氧化物類；乙烯基三甲氧基矽烷、乙 烯基三乙氧基矽烷、二甲氧基甲基乙烯基矽烷、二甲氧基乙基乙烯基矽烷、二乙氧基甲基乙烯基矽烷、二乙氧基乙基乙烯基矽烷、乙基甲基二乙烯基矽烷、甲基乙烯基二甲氧基矽烷、乙基乙烯基二甲氧基矽烷、甲基乙烯基二乙氧基矽烷、乙基乙烯基二乙氧基矽烷、對苯乙烯基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二甲氧基矽烷、3-甲基丙烯醯氧基丙基三甲氧基矽烷、3-甲基丙烯醯氧基丙基甲基二乙氧基矽烷、3-甲基丙烯醯氧基丙基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷等含聚合性雙鍵之矽烷烷氧化物；十甲基環五矽氧烷等環狀矽氧烷；單末端改質聚矽氧油、兩封端聚矽氧油、側鏈型聚矽氧油等改質(反應性)聚矽氧油；以及可列舉(甲基)丙烯酸、馬來酸、馬來酸酐等含羧基之單體等。
交聯性及非交聯性單體並不限定於上述例示列舉之單體，亦可為其他聚合性單體，例如公知之聚合性單體。
藉由公知之方法使上述具有乙烯性不飽和基之聚合性單體聚合，藉此可獲得上述樹脂粒子。作為該方法，例如可列舉於自由基聚合起始劑之存在下進行懸浮聚合之方法、及使用非交聯之種子粒子與自由基聚合起始劑一起使單體膨潤而進行聚合之方法(所謂之種子聚合法)等。該等聚合方法之條件並無特別限制，可設為公知之條件。
於上述基材為除金屬粒子以外之無機或有機無機混合樹脂之情形時，關於作為基材之材料之無機物，可列舉二氧化矽及碳黑等。該無機物較佳為非金屬。上述二氧化矽並無特別限定，例如可列舉藉由於使具有2個以上之水解性烷氧基矽基之矽化合物水解而形成交聯聚合物粒子後，視需要進行煅燒而獲得之粒子。作為上述有機無機混合樹脂，例如可列舉由經交聯之烷氧基矽基聚合物及丙烯酸樹脂形成之有機無機混合粒子等。於為基材粒子之情形時，可設為除金屬粒子以外之無機粒子或有機無機混合樹脂粒子。
作為上述基材之材料之其他例，可列舉包含聚輪烷之樹脂。聚輪烷係指鏈狀高分子貫通環狀分子之開口部而形成之結構。聚輪烷之種類並無特別限定，例如可列舉公知之聚輪烷。若為基材粒子，則可設為含聚輪烷之粒子。
於構成基材之材料為包含聚輪烷之樹脂之情形時，聚輪烷較佳為交聯體。具體而言，較佳為聚輪烷中之環狀分子與其他聚輪烷中之環狀分子以高分子鏈交聯而成之結構。若為此種交聯聚輪烷，則基材之柔軟性變高，故而容易發揮應力緩和效果，藉此於將燒結材料應用於連接結構體之情形時，容易抑制連接結構體之龜裂及翹曲之產生。即便為此種作為交聯體之聚輪烷，其種類亦並無特別限定，例如可列舉公知之交聯聚輪烷。
上述聚輪烷例如可藉由公知之方法進行製造。例如，藉由使具備具有聚合性官能基之環狀分子的聚輪烷與聚合性單體之混合物進行反應，而製造具有交聯結構之聚輪烷。該反應例如可藉由公知之方法進行。
具備具有聚合性官能基之環狀分子的聚輪烷之種類並無特別限制。若列舉具體例，則有由Advanced Soft Materials股份有限公司市售之「SeRM(註冊商標)Super Polymer SM3405P」、「SeRM(註冊商標)Key Mixture SM3400C」、「SeRM(註冊商標)Super Polymer SA3405P」、「SeRM(註冊商標)Super Polymer SA2405P」、「SeRM(註冊商標)Key Mixture SA3400C」、「SeRM(註冊商標)Key Mixture SA2400C」、「SeRM(註冊商標)Super Polymer SA3405P」、「SeRM(註冊商標)Super Polymer SA2405P」等。
關於基材粒子之平均粒徑，例如就確保燒結材料中之填充部3之優異分散性之觀點而言，可設為0.1μm以上且50以下。基材粒子之平均粒徑較佳為1μm以上，更佳為3μm以上，又，較佳為50μm以下，更佳為10μm以下。
以上所述之基材粒子之平均粒徑於形狀為真球狀之情形時，係指直徑，於為真球狀以外之形狀之情形時，係指最大徑與最小徑之平均值。而且，基材粒子之平均粒徑係指利用掃描式電子顯微鏡觀察基材粒子且利用游標卡尺測定隨機選擇之50個基材粒子之粒徑所得之平均值。再者，於基材粒子如上述般被其他材料被覆之情形時，其平均粒徑亦包含其被覆層。
基材粒子之粒徑之變異係數(CV值)例如為50%以下。上述變異係數(CV值)由下述式表示。
CV值(%)=(ρ/Dn)×100
ρ：粒子之粒徑之標準偏差
Dn：粒子之粒徑之平均值。
就容易使緩衝部2單分散化之觀點而言，基材粒子之CV值較佳為40%以下，更佳為30%以下。基材粒子之粒徑之CV值之下限並無特別限定。CV值可為0%以上，亦可為5%以上，亦可為7%以上，亦可為10%以上。
基材粒子之硬度例如可設為10N/mm2以上且3000N/mm2以下。就燒結材料之熱應力之緩和作用及接合強度兩者容易提昇之觀點而言，10%K值較佳為100N/mm2以上，更佳為1000N/mm2以上，較佳為2500N/mm2以下，尤佳為2000N/mm2以下。
此處所謂之10%K值係將基材粒子壓縮10%時之壓縮彈性模數。可以如下方式測定。首先，使用微小壓縮試驗機，利用圓柱(直徑50μm、金剛石製)之平滑壓頭端面，於25℃、歷時60秒負荷最大試驗負載20mN之條件下，將基材粒子壓縮。測定此時之負載值(N)及壓縮位移(mm)。根據所獲得之測定值，可藉由下述式求出上述壓縮彈性模數。
10%K值(N/mm2)=(3/21/2)‧F‧S-3/2‧R-1/2
F：粒子壓縮變形10%時之負載值(N)
S：粒子壓縮變形10%時之壓縮位移(mm)
R：粒子之半徑(mm)
微小壓縮試驗機係使用Fischer公司製造之「Fischerscope H-100」等。再者，於求30%K值之情形時，亦可藉由求出使粒子壓縮變形30%時之上述各參數而算出。
作為上述燒結促進劑或膠體觸媒，可列舉金屬微粒子或助熔劑(flux)成分。
作為上述金屬微粒子，可列舉金、銀、鉑、鈀、錫、銅、鍺、銦、鈀、鋅、銦、鋅、銥、銠、釕、鋨及該等之合金等。上述金屬微粒子可僅為1種，亦可包含2種以上。
作為將上述金屬微粒子配置於基材粒子表面上之方法，例如可列舉下述(1)~(3)。
(1)於基材粒子之分散液中添加金屬微粒子，藉由凡得瓦力使上述金屬微粒子集成、附著於上述基材粒子之表面的方法。
(2)於放入有基材粒子之容器中添加金屬微粒子，藉由因容器之旋轉等產生之機械作用使上述金屬微粒子附著於上述基材粒子之表面的方法。
(3)於基材粒子之分散液中添加金屬奈米膠體，藉由化學鍵結使上述金屬奈米膠體集成於上述基材粒子之表面後，利用還原劑將金屬奈米膠體還原而使之金屬化，藉此使金屬微粒子附著於基材粒子之表面的方法。
其中，就容易控制附著之金屬微粒子之量之觀點而言，較佳為上述(1)之方法。再者，即便為基材粒子以外之基材，亦可採用上述(1)~(3)之方法。
上述金屬微粒子之平均粒徑較佳為1nm以上，更佳為5nm以上，較佳為1000nm以下，更佳為500nm以下，進而較佳為100nm以下。再 者，於上述金屬微粒子使用上述(3)之方法中之金屬奈米膠體之情形時，較佳為1nm以上，更佳為5nm以上，較佳為50nm以下，更佳為40nm以下，進而較佳為35nm以下。若上述金屬微粒子之粒徑為上述下限以上及上述上限以下，則粒子與燒結體之接觸面積變大。上述金屬奈米膠體之徑係指最大徑。上述金屬微粒子之平均徑係藉由利用穿透式電子顯微鏡等進行觀察並對隨機抽選之100個金屬微粒子之最大徑進行平均而求出。
作為上述助熔劑成分，可列舉公知之助熔劑，例如可列舉樹脂系助熔劑、有機系助熔劑、無機系助熔劑等。作為樹脂系助熔劑，可列舉以松脂酸、長葉松酸(palustric acid)、脫氫松脂酸、異海松酸、新松脂酸、海松脂酸(pimaric acid)為主成分之松香。作為有機系助熔劑，可列舉脂肪族羧酸、芳香族羧酸。作為無機系助熔劑，可列舉溴化銨或氯化銨等鹵化物。上述助熔劑成分可僅為1種，亦可含有2種以上。藉由配置於基材粒子之助熔劑成分，於燒結過程中燒結體表面上之氧化被膜被去除，於基材粒子表面促進燒結反應，而使基材粒子與燒結體之接觸面積變大。
於複合體為被覆有金屬部之基材之情形時，作為基材之種類，與具有於基材配置有膠體觸媒或燒結促進劑之結構之複合體之情形相同。於該情形時，基材亦可為基材粒子。
上述金屬部由包含金屬之材料形成。作為該金屬，例如可例示金、銀、錫、銅、銅、鍺、銦、鈀、碲、鉈、鉍、鋅、砷、硒、鐵、鉛、釕、鋁、鈷、鈦、銻、鎘、矽、鎳、鉻、鉑、銠等。金屬部可僅為該等各金屬中之任一種，或者亦可包含2種以上。又，金屬部亦可為上述例示列舉之各金屬中之2種以上之金屬之合金。
金屬部例如可以被覆上述基材之方式層狀地形成。於該情形時，金屬部可由1層形成，或者亦可由多層形成。
金屬部之厚度例如可設為0.5nm以上，較佳為10nm以上，又，可設為10μm以下，較佳為1μm以下，進而較佳為500nm以下，尤佳為300nm以下。若金屬部之厚度為上述下限以上及上述上限以下，則作為填充部3之複合粒子容易於基部1中更均勻地分散，可使緩衝部2更均勻地分散。
於基材粒子之表面上形成金屬部之方法並無特別限定。作為形成金屬部之方法，例如可列舉利用無電解鍍覆之方法、利用電解鍍覆之方法、利用物理蒸鍍之方法、以及將金屬粉末或者含有金屬粉末及黏合劑之漿料塗佈於基材粒子之表面之方法等。就金屬部之形成較為簡單之觀點而言，較佳為利用無電解鍍覆之方法。作為上述利用物理蒸鍍之方法，可列舉真空蒸鍍、離子鍍覆及離子濺鍍等方法。
於金屬部為多層結構之情形時，亦可藉由相同之方法形成金屬部。例如，可藉由採用上述金屬部之形成方法於基材表面形成第1層金屬部，於該第1層表面進而依序形成下一層，藉此形成多層結構之金屬部。
上述金屬部亦可於外表面具有多個突起。突起例如可藉由公知之方法形成。突起之形狀及大小並無特別限定。例如，突起之剖面可為球狀或橢圓形狀，亦可形成為“如越朝向突起前端越尖之針狀”。
突起之平均高度可設為1nm以上且1000nm以下，較佳為5nm以上，更佳為50nm以上，較佳為900nm以下，更佳為500nm以下。若上述突起之平均高度為上述下限以上及上述上限以下，則複合體(例如，複合粒子)容易與作為燒結體之基部1接觸。
突起之平均高度例如可以如下方式測定。以複合體(例如，複合粒子)之含量成為30重量%之方式添加至Kulzer公司製造之「Technovit4000」，並使之分散，而製作複合體檢查用嵌入樹脂。以通過該檢查用嵌入樹脂中之分散之複合體之中心附近之方式使用離子研磨裝置(Hitachi High-Technologies公司製造之「IM4000」)，切出複合體之剖面。然後，使用場發射型掃描式電子顯微鏡(FE-SEM)，設定為影像倍率5萬倍，隨機選擇20個複合體，觀察各複合體之突起50個。將自突起之底面至突起之頂部之高度設為突起之高度，進行算術平均而設為上述突起之平均高度。
突起底面之平均徑可設為3nm以上且5000nm以下，較佳為50nm以上，更佳為80nm以上，較佳為1000nm以下，更佳為500nm以下。此處所謂之突起底面之平均徑係指以與上述突起之平均高度之測定方法相同之順序，藉由使用嵌入樹脂之FE-SEM觀察，分別觀察隨機選擇之20個複合粒子之突起，計測各基部之兩端間距離，對其等進行算術平均而求出之值。
複合體具有於上述基材之表面之一部分或全部配置有膠體觸媒或燒結促進劑之結構。或者，複合體具有於上述基材之表面之一部分或全部被覆有金屬部之結構。於複合體為複合粒子之情形時，具有於基材粒子之表面之一部分或全部配置有膠體觸媒或燒結促進劑之結構。或者，複合粒子具有於上述基材之表面之一部分或全部被覆有金屬部之結構。
作為複合粒子之其他形態，亦可具備具有凹部之基材粒子及配置於基材粒子之表面上之膠體觸媒或金屬部。於該形態之複合粒子中，亦可於凹部被覆膠體觸媒或金屬部。
製備具有凹部之基材粒子之方法並無特別限定。例如，可藉由對基材粒子進行後處理，而於基材粒子形成凹部。利用後處理之凹部之形成方法並無特別限定，例如，可採用公知之方法。具體而言，可列舉對基材粒子之表面進行蝕刻處理之方法、於氧氣氛圍下進行電漿處理、臭氧處理及加熱處理之方法、進行加濕處理之方法、於真空中進行熱處理之方法、於加壓及加濕條件下進行熱處理之方法、利用氧化劑進行濕式處理之方法、利用球磨機等進行物理處理之方法等。
凹部之平均深度並無特別限定。例如，凹部之平均深度可設為基材粒子之平均半徑之0.1%以上且80%以下。再者，此處所謂之凹部之深度表示將具有凹部之基材粒子當作球狀時，從該球狀之基材粒子之表面至成為凹部之最底面之點的距離。具體而言，係指以與上述突起之平均高度之測定方法相同之順序，藉由使用嵌入樹脂之FE-SEM觀察，分別觀察隨機選擇之20個複合粒子之凹部，對各凹部之深度進行算術平均而求出之值。
於複合粒子具有凹部之情形時，複合粒子容易對變形進行追隨，其結果，燒結材料之熱應力之緩和作用及接合強度進一步提昇。
用以形成填充部3之粒子之形狀並無特別限定。作為粒子之形狀，例如可列舉球狀、橢圓狀、不定形狀、針狀、棒狀、板狀、鱗片狀等。就填充部3容易均勻地分散於基部1之方面而言，作為粒子之形狀，較佳為球狀或橢圓狀。又，如上述般，就基部1容易以於特定之一維方向具有配向性之方式分佈而存在之觀點而言，粒子之形狀較佳為針狀、棒狀、板狀。
關於形成填充部3之粒子之平均粒徑，例如就確保作為燒結體之基部1中之填充部3之分散性之觀點而言，可設為0.1μm以上且50μm以下。粒子之平均粒徑較佳為1μm以上，更佳為3μm以上，又，較佳為10μm以下。
於填充部3由纖維形成之情形時，纖維之種類並無特別限定。作為纖維，例如除天然纖維、合成纖維以外，還可列舉玻璃纖維、碳纖維、岩石纖維。天然纖維可例示纖維素、絹、棉、羊毛、麻。合成纖維可例示聚對苯二甲酸乙二酯等聚酯、聚醯胺、聚醯亞胺、丙烯酸、聚烯烴、聚甲基戊烯、聚芳酯、聚縮醛、聚苯醚、聚碸、聚醚醚酮、聚苯硫醚。
製造具有上述結構之燒結材料之方法並無特別限制。例如，可藉由公知之方法製造燒結材料。
例如，可藉由以含有用以形成基部1之金屬、用以形成緩衝部2 之材料、及用以形成填充部3之粒子及/或纖維之接合用組成物作為燒結用原料，並將該接合用組成物進行燒結，而獲得燒結材料。再者，於獲得緩衝部2僅由孔隙形成之燒結材料之情形時，接合用組成物不含第2原料。以下，將用以形成基部1之金屬稱為「第1原料」，將用以形成緩衝部2之材料稱為「第2原料」，將用以形成填充部3之粒子及/或纖維稱為「第3原料」。
第1原料只要為可形成基部1之燒結體之金屬原料，則並無特別限制。例如，第1原料可設為金屬粒子。金屬粒子可為金屬單質粒子，或者亦可為金屬化合物之粒子。金屬化合物係含有金屬原子及該金屬原子以外之原子之化合物。
作為金屬化合物之具體例，可列舉金屬氧化物、金屬之碳酸鹽、金屬之羧酸鹽及金屬之錯合物等。金屬化合物較佳為金屬氧化物。例如，上述金屬氧化物係於還原劑之存在下藉由連接時之加熱成為金屬粒子後進行燒結。上述金屬氧化物係金屬粒子之前驅物。作為金屬之羧酸鹽粒子，可列舉金屬之乙酸鹽粒子等。
第1原料之金屬可例示選自由金、銀、錫、銅、鍺、銦、鈀、碲、鉈、鉍、鋅、砷、硒及含有該等金屬元素中至少1種金屬元素之合金所構成之群中1種以上。
於第1原料為粒子形狀之情形時，其平均粒徑可設為10nm以上且10μm以下。又，第1原料亦可含有平均粒徑不同之2種以上，於該情形時，可使燒結材料之接合強度提昇。例如，平均粒徑較小之金屬粒子的平均粒徑可設為10nm以上且100nm以下，平均粒徑較大之金屬粒子的平均粒徑可設為1μm以上且10μm以下。平均粒徑較大之第1原料相對於平均粒徑較小之第1原料的調配量之比可設為1/9以上且9以下。再者，上述平均粒徑係藉由利用掃描式電子顯微鏡觀察金屬粒子，對所觀察之影像中任意選擇之50個各粒子之最大 徑進行算術平均而求出。
於第1原料為金屬氧化物之粒子之情形時，亦可併用還原劑。作為還原劑，可使用公知之還原劑。還原劑之含量相對於第1原料100重量份，較佳為1重量份以上，更佳為10重量份以上，較佳為1000重量份以下，更佳為500重量份以下，進而較佳為100重量份以下。若上述還原劑之含量為上述下限以上，則容易獲得緻密之燒結體。
第1原料中亦可視需要包含其他成分。作為其他成分，例如可列舉熱塑性樹脂或硬化性樹脂。作為硬化性樹脂，例如可列舉公知之光硬化性樹脂及熱硬化性樹脂。光硬化性樹脂亦可含有光硬化性樹脂及光聚合起始劑。熱硬化性樹脂亦可含有公知之熱硬化性樹脂及熱硬化劑。
第1原料中亦可含有分散介質。作為分散介質，例如可列舉公知之溶劑等。
第1原料亦可使用市售之製品。作為具體例，可列舉Kyocera Chemical公司製造之「CT2700」、Heraeus公司製造之「ASP295」、「ASP016」、「ASP043」、Henkel公司製造之「LOCTITE ABLESTIK SSP2020」、Namics公司製造之「H9890-6A」、哈利瑪化成公司製造之「NH-4000」、「NH-225D」、「NH-3000D」、Kaken-Tech公司製造之「CM-3212」、「CR-3520」、Nihon superior公司製造之「Alconano Ag Paste ANP-1」等。
第1原料較佳為具有藉由未達400℃之加熱進行燒結之性質，更佳為350℃以下，較佳為300℃以上。若第1原料之燒結之溫度為上述上限以下或未達上述上限，則可有效率地進行燒結，可進而減少燒結所需之能量且減小環境負荷。
第1原料可僅使用1種，或者亦可併用2種以上而使用。
於緩衝部2非孔隙之情形時，使用第2原料。第2原料可使用不同於第1原料之材料。作為第2原料，與用以形成上述緩衝部2之材料相同。於第2原料為金屬之情形時，係指與第2原料中所含之金屬不同種類之金屬元素。
第3原料與用以形成上述填充部3之粒子及/或纖維相同。
第3原料較佳為含有上述複合體。於該情形時，於所獲得之燒結材料中，填充部3與作為燒結體之基部1的親和性提高，因此填充部3容易更均勻地分散於燒結材料中。其結果，緩衝部2亦容易於燒結材料中均勻地分散(單分散化)，峰度A進一步變大，尤其可提昇燒結材料之熱應力之緩和作用及接合強度之兩者。若複合體為複合粒子，則進而較佳。
第3原料可僅使用1種，或者亦可併用2種以上而使用。
於接合用組成物(燒結用原料)中，第1原料、第2原料、第3原料之混合比率並無特別限定。例如，於使用接合用組成物形成燒結材料之情形時，較佳為以填充部之含量成為0.01重量%以上且10重量%以下之方式調節第1原料、第2原料、第3原料之含量。再者，只要不阻礙本發明之效果，則接合用組成物可含有其他原料。接合用組成物亦可僅由第1原料、第2原料、第3原料構成。
使接合用組成物燒結之方法並無特別限定。燒結溫度可設為100℃以上且400℃以下。如下所述，於在加壓下進行燒結之情形時，燒結溫度較佳為150℃以上且350℃以下。又，於不在加壓下進行燒結之情形時，燒結溫度較佳為200℃以上且350℃以下。
燒結時間例如可設為30秒以上且7200秒以下。如下所述，於在加壓下進行燒結之情形時，燒結時間較佳為180秒以上且600秒以下。又，於不在加壓下進行燒結之情形時，燒結時間較佳為180秒以上且5400秒以下。再者，燒結時間根據燒結溫度進行調整即可，例如若設為更高溫並縮短燒結時 間，則生產效率優異。
燒結亦可在加壓下進行。該情形時之壓力可設為0.1~20MPa。
燒結可於空氣氛圍下進行，亦可於氮氣等非活性氣體氛圍下進行。
就容易觀察上述三維影像之觀點而言，較佳為於在金屬板上塗佈接合用組成物之狀態下進行燒結。作為金屬板，例如可列舉銅基板。塗佈之方法例如為網版印刷法。燒結時，亦可於網版塗佈之接合用組成物之表面進而載置其他金屬板，於夾入有接合用組成物之狀態下進行燒結。
於接合用組成物被燒結而形成燒結體(基部1)之過程中，由於存在第3原料(即，成為填充部3之原料)，故而緩衝部2(例如孔隙)不易偏集存在於燒結體中而容易均勻地分散。藉此，達成緩衝部2之單分散化，基部1之體積分佈亦調整為適當之範圍，燒結材料之峰度A變大。
如上述般，藉由包括將接合用組成物燒結之步驟之製造方法，而可獲得燒結材料。針對以此方式製造之燒結材料，可依據上述順序來計測燒結材料之峰度A。
另一方面，用以計測峰度B之燒結材料即經去除填充部3之燒結材料(以下，有時稱為「空白燒結材料」)例如可以如下方式製造。
藉由自上述接合用組成物去除第3原料後進行燒結，而可獲得空白燒結材料。於該情形時，將第1原料、第2原料之種類及使用量以及燒結條件設為與獲得用以計測峰度A之燒結材料之方法相同之條件。再者，作為第3原料之去除方法，例如可列舉取接合用組成物，利用光學顯微鏡進行觀察，利用玻璃毛細管自其中去除第3原料之方法或藉由離心分離去除第3原料之方法。或者，於上述燒結材料之製造方法中，使用不含第3原料之接合用組成物進行燒結，藉此可獲得空白燒結材料。於該情形時，亦將第1原料、第2原料之種類及 使用量以及燒結條件設為與獲得用以計測峰度A之燒結材料之方法相同之條件。
本發明之接合用組成物尤佳為含有下述之複合體及金屬粒子，該複合體為：具有於上述基材配置有膠體觸媒或燒結促進劑之結構、或者具有基材被覆有金屬部之結構、以及金屬粒子。即，於接合用組成物中，較佳為第1原料含有上述金屬粒子，第3原料含有上述複合體。於該情形時，容易達成緩衝部2之單分散化，基部1之體積分佈亦容易調整為適當之範圍，燒結材料之峰度A變大。再者，第1原料、第3原料及其混合比率等之較佳態樣如上所述。
若使本發明之接合用組成物燒結而形成燒結材料，則可滿足A>B。或者，此種接合用組成物之燒結材料之A之值可成為0.2以上。其結果，燒結材料之熱應力之緩和作用及接合強度兩者變得更優異，例如適宜作為用以將半導體元件接合之接合構件。
為確認接合用組成物之燒結材料可滿足A>B或可滿足A≧0.2，將接合用組成物於下述條件下進行燒結。
首先，將接合用組成物以成為100μm之厚度之方式網版塗佈於厚度1mm之Cu基板上，使其表面被厚度1mm之Cu基板夾住。將該夾入之接合用組成物於130℃下且於氮氣氛圍下乾燥90秒鐘，繼而，一面以5MPa進行加壓，一面於300℃下加熱3分鐘。藉此獲得燒結材料，因此可使用該燒結材料計測A。又，藉由上述方法自接合用組成物去除第3原料(複合體)，而製備用以測定B之組成物，使用該組成物進行與A之計測相同之方法，藉此可計測B。
本發明之燒結材料之熱應力之緩和作用及接合強度兩者更優異。因此，本發明之燒結用材料可應用於連接結構體之連接部。於連接部具有本發明之燒結用材料的連接結構體其熱應力之緩和作用優異，因此成為耐久性優異之結構體。尤其是，連接部含有由本發明之燒結用材料形成之接合構件， 因此接合強度亦優異。
連接結構體之種類並無特別限定。例如，可列舉各種半導體裝置(功率裝置)。連接結構體之結構例如亦可設為與公知相同。
又，上述複合體作為用以形成燒結材料之添加劑尤其有效。其原因在於：具備上述複合體作為填充部3之燒結材料容易於燒結材料中分散，因此容易有助於緩衝部2之均勻分散化(單分散化)。複合體更佳為複合粒子。
因此，上述複合體適宜作為用以形成上述燒結材料之填充部之添加劑(緩衝部分佈調節劑)。即，上述複合體(例如，複合粒子)適合用於使基部1及緩衝部2分佈，適合用於製造燒結材料。
又，使用含有上述第1原料、第2原料及第3原料之接合用組成物獲得燒結材料之方法亦適宜作為調節形成於燒結材料之基部1及緩衝部2的分佈狀態之方法。
[實施例]
以下，藉由實施例更具體地說明本發明，但本發明並不限定於該等實施例之態樣。
(實施例1)
作為基材粒子，準備粒徑為3.0μm之二乙烯苯共聚物樹脂粒子(積水化學工業公司製造之「Micropearl SP-203」)。
使用超音波分散器使基材粒子A 10重量份分散於含有鈀觸媒液5重量%之鹼性溶液100重量份中後，藉由對溶液進行過濾而提取基材粒子A。繼而，將基材粒子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之表面活化。將表面經活化之基材粒子A充分水洗後，添加至蒸餾水500重量份中，使之分散，藉此獲得懸浮液(A)。
將懸浮液(A)放入至含硫酸銅20g/L及乙二胺四乙酸30g/L之溶液中，而獲得粒子混合液(B)。
又，作為無電解鍍銅液，準備鍍銅液(C)，該鍍銅液(C)係利用氨將含有硫酸銅250g/L、乙二胺四乙酸150g/L、葡萄糖酸鈉100g/L、及甲醛50g/L之混合液調整為pH值10.5者。
又，作為無電解鍍銀液，準備鍍銀液(D)，該鍍銀液(D)係利用氨將含有硝酸銀30g/L、琥珀醯亞胺100g/L、及甲醛20g/L之混合液調整為pH值8.0者。
於調整為55℃之分散狀態之粒子混合液(B)中緩慢滴加上述鍍銅液(C)，而進行無電解鍍銅。鍍銅液(C)之滴加速度為30mL/分鐘，滴加時間為30分鐘，而進行無電解鍍銅。以此方式獲得粒子混合液(E)，該粒子混合液(E)為含有於樹脂粒子之表面具備銅金屬部作為第1金屬部之粒子者。
其後，藉由對粒子混合液(E)進行過濾而提取粒子，並進行水洗，藉此獲得於上述基材粒子A之表面上配置有銅金屬部之粒子。將該粒子充分水洗後，添加至蒸餾水500重量份中，使之分散，藉此獲得粒子混合液(F)。
其次，於調整為60℃之分散狀態之粒子混合液(F)中緩慢滴加上述鍍銀液(D)，而進行無電解鍍銀。鍍銀液(D)之滴加速度為10mL/分鐘，滴加時間為30分鐘，而進行無電解鍍銀。其後，藉由進行過濾而提取粒子，並進行水洗及乾燥，藉此獲得於基材粒子A之表面上具備依序積層銅及銀而成之金屬部(金屬部整體之厚度：0.1μm)的複合粒子A。
將作為第1原料之銀漿料(Nihon superior公司製造之「Alconano Ag Paste ANP-1」)0.98g及上述複合粒子A 0.02g利用刮勺進行混練以充分分 散，而製備接合用組成物。
將經混練之接合用組成物以成為100μm之厚度之方式網版塗佈於厚度1mm之Cu基板上，使其表面被厚度1mm之Cu基板夾入。將該夾入之接合用組成物於130℃下且於氮氣氛圍下乾燥90秒鐘，繼而，一面以5MPa進行加壓，一面於300℃下加熱3分鐘，藉此獲得燒結材料。燒結材料中，複合粒子之含量為2重量%，複合粒子間之最接近距離為3.52μm。
針對所獲得之燒結材料，使用FEI製之「Helios660」，藉由FIB-SEM法進行斷層攝影，並重建該影像，而獲得燒結材料之三維影像。作為觀察條件，於加速電壓2kV下設為反射電子像，且將試樣傾斜52°。
圖2(a)表示實施例1中所獲得之三維影像，表示整體影像及三個斷層攝影像(剖面影像)。又，如圖2(b)所示，圖2(a)之三維影像係將燒結材料劃分為125個區塊中之一個區塊。
如圖2(a)所示，所獲得之燒結材料顯示出3種不同之對比度，確認形成有基部1、緩衝部2及填充部3。基部1係銀漿料之燒結體(銀燒結體)，填充部3係複合粒子。又，於本實施例中，緩衝部2係孔隙。
使用FEI公司製造之「AVIZO」算出所獲得之125個區塊各自之基部1、緩衝部2、填充部3之體積，並製成體積分佈，根據該體積分佈算出峰度A，結果為0.97。
另一方面，準備自上述實施例1之接合用組成物去除了複合粒子之組成的接合用組成物，而製成峰度B測定用之接合用組成物。
將所獲得之峰度B測定用之接合用組成物以成為100μm之厚度之方式網版塗佈於厚度1mm之Cu基板上，使其表面被厚度1mm之Cu基板夾入。將該夾入之接合用組成物於130℃下且於氮氣氛圍下乾燥90秒鐘，繼而，一面以5MPa進行加壓，一面於300℃下加熱3分鐘，藉此獲得燒結材料。藉由 與峰度A相同之方法計測該燒結材料之峰度B，結果為0.52。
(熱應力之緩和作用及接合強度評價)
熱應力之緩和作用及接合強度係基於「JIS Z 3198-7：無鉛焊錫試驗方法-第7部晶片零件之焊接接頭剪切試驗方法」中記載之「焊接接頭剪切試驗方法」進行評價。
圖3係示意性地表示用以測定熱應力之緩和作用及接合強度之測定裝置。於該測定中，使用圓筒狀之銅(徑10mm且厚5mm)作為基板100。於基板100上塗佈各實施例及比較例中獲得之任一種接合用組成物而形成漿料層(徑5mm且厚50μm)。然後，於該漿料層上配置銅製之圓盤晶片101(徑5mm且厚2mm)，一面以5MPa進行加壓，一面於300℃下燒結3分鐘，藉此利用燒結材料將基板100與晶片101接合。將其安設於剪切強度試驗機105，以剪切速度6mm/min對晶片101及接合部施加負載，將位移與負載之關係圖表化而獲得應力-應變曲線，計測表現為熱應力之功及接合強度。表現為熱應力之功可藉由算出應力-應變曲線中位移開始後至斷裂點為止之積分值而進行計測，係表示直至斷裂為止所吸收之能量者。接合強度係應力-應變曲線中斷裂點之應力值。
使用實施例1之接合用組成物進行熱應力之緩和作用及接合強度之評價，結果表現為熱應力之功為0.988J，接合強度為85.04MPa，可知可賦予較以往優異之熱應力之緩和作用及接合強度。
(實施例2)
將作為第1原料之銀漿料變更為0.99g，將上述複合粒子A變更為0.01g，除此以外，藉由與實施例1相同之方法製備接合用組成物。複合粒子之含量為1重量%。針對所獲得之接合用組成物，藉由與實施例1相同之方法製作燒結材料，並藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱 應力之功、斷裂伸長率及接合強度。
(實施例3)
將作為第1原料之銀漿料變更為0.90g，將上述複合粒子A變更為0.10g，除此以外，藉由與實施例1相同之方法製備接合用組成物。複合粒子之含量為10重量%。針對所獲得之接合用組成物，藉由與實施例1相同之方法製作燒結材料，並藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度。
(實施例4)
將作為第1原料之銀漿料變更為Kyocera Chemical公司製造之放入有樹脂之銀漿料「CT2700」0.98g，除此以外，藉由與實施例1相同之方法製備接合用組成物。複合粒子之含量為2重量%。將所獲得之接合用組成物以成為100μm之厚度之方式網版塗佈於厚度1mm之Cu基板上，使其表面經厚度1mm之Cu基板夾入。藉由將該夾入之接合用組成物於200℃下加熱90分鐘而獲得燒結材料。藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度。
(實施例5)
使用作為纖維之「L-MWNT-4060(NTP公司製造)」0.02g代替複合粒子A，除此以外，藉由與實施例1相同之方法製備接合用組成物。纖維之含量為2重量%。針對所獲得之接合用組成物，藉由與實施例1相同之方法製作燒結材料，並藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度。
(比較例1)
僅將作為第1原料之銀漿料(Nihon superior公司製造之「Alconano Ag Paste ANP-1」)作為接合用組成物。針對所獲得之接合用組成物，藉由與實施例1 相同之方法製作燒結材料，並藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度。
(比較例2)
僅將作為第1原料之銀漿料(Kyocera Chemical公司製造之「CT2700」)作為接合用組成物。針對所獲得之接合用組成物，藉由與實施例1相同之方法製作燒結材料，並藉由與上述方法相同之方法分別測定該燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度。
表1係使用各實施例及比較例中獲得之接合用組成物製作之燒結材料之峰度A、峰度B、表現為熱應力之功、斷裂伸長率及接合強度之評價結果的統整。
Figure 107105793-A0202-12-0031-3
根據表1可知，於使用實施例2~5之接合用組成物之情形時，亦可賦予較以往優異的熱應力之緩和作用及接合強度(均為45MPa以上)。
於任一實施例中，均可賦予優異的熱應力之緩和作用及接合強度，可以說其原因在於：在滿足A>B之基礎上，進而填充部3(複合粒子A或纖維)與基部1(銀燒結體)形成有化學鍵(例如金屬鍵)。
1‧‧‧基部
2‧‧‧緩衝部
3‧‧‧填充部

Claims (11)

  1. 一種燒結材料，其具備基部、緩衝部及填充部，上述基部係金屬之燒結體，上述緩衝部及填充部分散存在於上述基部中，上述緩衝部由孔隙及不同於上述燒結體之材料中至少任一者形成，上述填充部由粒子及纖維中至少任一者形成，於將上述燒結材料之三維影像中之上述基部之體積分佈之峰度設為A，且將經去除上述填充部之上述燒結材料之三維影像中之基部之體積分佈之峰度設為B時，滿足A>B。
  2. 一種燒結材料，其具備基部、緩衝部及填充部，上述基部係金屬之燒結體，上述緩衝部及填充部分散存在於上述基部中，上述緩衝部由孔隙及不同於上述燒結體之材料中至少任一者形成，上述填充部由粒子及纖維中至少任一者形成，於將上述燒結材料之三維影像中之上述基部之體積分佈之峰度設為A時，A之值為0.2以上。
  3. 如申請專利範圍第1項之燒結材料，其中，A-B之值為0.1以上。
  4. 如申請專利範圍第1至3項中任一項之燒結材料，其中，上述填充部之含量為0.01重量%以上且10重量%以下。
  5. 如申請專利範圍第1至3項中任一項之燒結材料，其中，上述填充部彼此之最接近距離為1μm以上且10μm以下。
  6. 如申請專利範圍第1至3項中任一項之燒結材料，其中，上述基部以於一維方向具有配向性之方式分佈而存在。
  7. 一種連接結構體，其於連接部具有申請專利範圍第1至6項中任一項之燒結材料。
  8. 一種複合粒子，係為了形成申請專利範圍第1至6項中任一項之燒結材料的填充部而使用，具有下述之結構：於基材粒子配置有膠體觸媒或燒結促進劑之結構、或者於基材粒子被覆有金屬部之結構。
  9. 一種接合用組成物，其含有下述之複合體及金屬粒子，該複合體為：具有於基材配置有膠體觸媒或燒結促進劑之結構、或者具有於基材被覆有金屬部之結構，於將上述接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為A，且將經去除上述複合體之接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為B時，滿足A>B。
  10. 一種接合用組成物，其含有下述之複合體及金屬粒子，該複合體為：具有於基材配置有膠體觸媒或燒結促進劑之結構、或者具有於基材被覆有金屬部之結構，於將上述接合用組成物之燒結材料的三維影像中之基部之體積分佈之峰度設為A時，A之值為0.2以上。
  11. 一種燒結材料之製造方法，其包括將申請專利範圍第9或10項之接合用組成物進行燒結之步驟。
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