TW202242910A - 接合構造體 - Google Patents

接合構造體 Download PDF

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Publication number
TW202242910A
TW202242910A TW111112164A TW111112164A TW202242910A TW 202242910 A TW202242910 A TW 202242910A TW 111112164 A TW111112164 A TW 111112164A TW 111112164 A TW111112164 A TW 111112164A TW 202242910 A TW202242910 A TW 202242910A
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Taiwan
Prior art keywords
joined
joint
ratio
joining
bonding
Prior art date
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TW111112164A
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English (en)
Inventor
山内真一
穴井圭
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日商三井金屬鑛業股份有限公司
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Publication of TW202242910A publication Critical patent/TW202242910A/zh

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    • B22F7/00—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
    • 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
    • B22F7/08—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 with one or more parts not made from powder
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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
    • 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

接合構造體(1)係由2個被接合材(11、12)及相鄰地形成於該等被接合材之間之接合部(15)接合而成。接合部(15)由以銅為主體之材料構成。於接合構造體(1)之厚度方向(Z)上剖面觀察時，該接合構造體之端部區域(A2)中之被接合材與接合部之接合比率(Rs)相對於該接合構造體之中央區域(A1)中之被接合材與接合部之接合比率(Rc)之比(Rs/Rc)為0.6以上0.9以下。接合比率(Rc)為0.3以上。

Description

接合構造體
本發明係關於一種接合構造體。
伴隨著近年來世界性之節能趨勢，作為變流器等電力轉換、控制裝置，被稱為功率裝置之半導體裝置得到廣泛使用。作為可應用於此種裝置之技術，本申請人提出了一種接合構造，其係由包含銅且具有規定化學結構之接合部連接2個被接合材而成者(參照專利文獻1)。 [先前技術文獻] [專利文獻]
專利文獻1：國際公開第2020/032161號說明書
專利文獻1中記載之接合構造可表現出高接合強度，但例如於將具備該接合構造之半導體裝置用於汽車用途等時，要求即使長期置於溫度變化劇烈之環境中，亦保持高接合強度，即要求高接合可靠性。
本發明之問題在於提供一種具有高接合可靠性之接合構造體。
本發明提供一種接合構造體，其係由2個被接合材及相鄰地形成於該等被接合材之間之接合部接合而成者， 上述接合部由以銅為主體之材料構成， 於上述接合構造體之厚度方向上剖面觀察時，該接合構造體之端部區域中之上述被接合材與上述接合部之接合比率Rs相對於該接合構造體之中央區域中之上述被接合材與上述接合部之接合比率Rc之比(Rs/Rc)為0.6以上0.9以下，且 上述接合比率Rc為0.3以上。
以下基於其較佳之實施方式說明本發明之接合構造體。
圖1(a)及(b)中示出了本發明之接合構造體之一實施方式。於該圖所示之實施方式中，接合構造體1具有第1被接合材11(以下，亦將其簡稱為「被接合材11」)及第2被接合材12(以下，亦將其簡稱為「被接合材12」)，並具有相鄰地形成於該等被接合材11、12之間之接合部15。接合構造體1中之被接合材11、12介隔接合部15而被接合，各被接合材11、12與接合部15之間未介置其他構件。該圖所示之實施方式之接合構造體1形成為接合部15及第1被接合材11以該順序積層於第2被接合材12之一個表面上之狀態。
圖1(a)及(b)所示之被接合材11被構成為其尺寸較被接合材12小，但並不限於該形態，可為各被接合材11、12彼此之尺寸相同，亦可構成為被接合材11較被接合材12大。進而，該圖所示之各被接合材11、12以及接合部15均為平面，但亦可根據需要形成為曲面。
又，圖1(a)及(b)所示之接合部15形成為其周緣較被接合材11之周緣更向外側延出，但並不限於該形態，亦可以接合部15之周緣與被接合材11之周緣相一致之狀態形成。
各被接合材11、12之種類沒有特別限制，但較佳為各被接合材11、12中之至少一者之與接合部15接觸之面包含金屬，更佳為被接合材11、12二者之與接合部15接觸之面均包含金屬。於該情形下，2個被接合材11、12亦較佳為介隔接合部15電性連接。即，各被接合材11、12分別獨立，較佳為導電體。作為形成各被接合材11、12之表面之金屬，就提高導電性之觀點而言，可分別獨立地較佳地舉出金、銀、銅、鎳及鈦中之至少一種。
作為包含上述金屬之各被接合材11、12，可分別獨立地舉出例如包含上述金屬之間隔件、散熱板、半導體元件以及表面具有上述金屬中之至少一種之基板等。作為基板，例如可使用於陶瓷或氮化鋁板之表面具有銅等金屬層之絕緣基板等。於使用半導體元件作為被接合材之情形時，半導體元件包含Si、Ga、Ge、C、N、As等元素中之一種以上。被接合材11、12之表面中存在之金屬可為金屬單質，或者亦可為2種以上之金屬之合金。 被接合材11較佳為間隔件、散熱板或半導體元件中之任一者。被接合材12較佳為基板。
接合部15係包含銅作為主體之構造體，相鄰地介置於被接合材11、12之間，較佳為介置於俯視全域中。接合部15較佳為包含50質量%以上之銅，更佳為包含60質量%以上之銅。接合部中之銅之含量可藉由以接合構造體1之厚度方向上之剖面為對象，利用能量分散型X射線光譜法(EDX)進行分析來測定。 關於此種接合部15，例如如後述之製造方法所示，可將含有包含銅之金屬粒子之組合物與兩個被接合材一同焙燒，而形成為金屬粒子彼此之燒結體。作為含有此種粒子而形成之燒結體之接合部15可於其構造中具有多個孔隙。
本發明之接合構造體之特徵之一在於，於厚度方向上剖面觀察時，被接合材與接合部之接合比率於接合構造體之中央區域及端部區域相互不同。
詳細而言，如圖1(a)所示，於使接合構造體1之各被接合材11、12與接合部15接合之最大區域A0之俯視時之圖心與將最大區域A0之平面面積縮小至50%而得之相似形之俯視時之圖心一致時，將該相似形之俯視形狀所表示之虛擬區域V1設為接合構造體1之中央區域A1。並且，將於厚度方向Z上剖面觀察接合構造體1之中央區域A1時，位於上述中央區域A1中之至少一個被接合材11、12與接合部15之界面處之接合比率設為第1接合比率Rc(以下，亦將其簡稱為「接合比率Rc」)。 再者，最大區域A0係沿著厚度方向Z觀察接合構造體1時，2個被接合材11、12及接合部15均存在之部位之最大區域。因此，當以圖1(a)及(b)所示之接合構造體1為例時，最大區域A0與被接合材11之俯視時之配置區域一致。
又，如圖1(a)所示，於俯視接合構造體1時，使最大區域A0之俯視時之圖心與將最大區域A0之平面面積縮小至90%而得之相似形之俯視時之圖心一致時，考慮到以該相似形之俯視形狀表示之虛擬區域V2。此時，當俯視接合構造體1時，將位於該虛擬區域V2之外側並位於較最大區域A0之周緣(相當於該圖中被接合材11之周緣11e)靠內側之區域設為接合構造體1之端部區域A2。並且，將於厚度方向Z上剖面觀察接合構造體1之端部區域A2時，位於上述端部區域A2中之至少一個被接合材11、12與接合部15之界面處之接合比率設為第2接合比率Rs(以下，亦將其簡稱為「接合比率Rs」)。成為接合比率Rs之對象之界面係與作為接合比率Rc之對象之界面相同之界面。
此時，接合比率Rs相對於接合比率Rc之比(Rs/Rc)較佳為0.6以上，更佳為0.7以上。又，Rs/Rc較佳為0.9以下，更佳為0.8以下。即，接合構造體1係於至少一個被接合材與接合部之界面處，中央區域A1之接合比率較端部區域A2之接合比率高者。
關於因Rs/Rc處於上述範圍內，故接合構造體可表現出高接合可靠性之理由，本發明人推測如下。於以下之說明中，以圖1所示之符號為例進行說明。 於2個被接合材11、12之間形成有接合部15之接合構造體1典型的是使用具有流動性之導電性組合物作為接合部15之形成材料，一面於將該組合物配置於2個被接合材11、12之間之狀態下進行加壓，一面於加快升溫速度之狀態下進行焙燒來製作。此時，組合物於焙燒初期還保留有流動性，故而藉由加壓，組合物被擠出而位於被接合材11、12之周緣外側，或者以於被接合材11、12之俯視中央區域A1中組合物之密度升高之方式移動。藉由於該狀態下燒結，於俯視中央區域A1中形成相對緻密之構造，並且組合物有效率地燒結，充分表現出與被接合材11、12之密接性之接合部15於各被接合材11、12之間形成於該被接合材11、12之俯視全域中。尤其當Rs/R處於上述特定範圍內時，可在維持整個接合構造體1之接合強度之同時，緩和接合構造體1之端部區域A2中之應力集中，因此即使於溫度變化之環境中，亦可維持接合部之高接合功能，從而可維持高接合可靠性。 與此相對，於在加壓不充分之條件或升溫速度不適當之條件下形成接合部15之情形時，位於接合構造體1之俯視中央區域A1中之接合部15難以形成為緻密構造，且Rs/Rc成為接近1之值。如此，無法緩和接合部15之端部區域A2中之應力集中，難以維持接合可靠性。
接合比率Rc較佳為0.3以上，更佳為0.4以上，進而較佳為0.5以上，就表現出與被接合材之充分之接合強度這一點而言，越高越佳。
接合比率Rs較佳為0.35以上0.6以下，更佳為0.35以上0.55以下，進而較佳為0.35以上0.5以下。接合比率Rs達到此種比率，從而使接合體之端部區域A2之彈性模數適當降低，因此可防止應力集中於端部區域A2而發生破裂。
上述之比Rs/Rc、第1接合比率Rc及第2接合比率Rs係規定至少一個被接合材11、12與接合部15之至少一個界面處之關係者，較佳為至少在被接合材11與接合部15之界面G1處滿足上述之比及各接合比率，此外，更佳為在被接合材12與接合部15之界面G2處亦同樣滿足上述較佳範圍。 此種接合構造體1例如如後述之製造方法所示，可藉由將含有包含銅之金屬粒子之導電性組合物與2個被接合材11、12一同於施加規定之壓力之狀態下，以規定之升溫速度進行焙燒而獲得。
第1接合比率Rc及第2接合比率Rs可用以下方法進行測定。 首先對測定對象之接合構造體1進行樹脂包埋之後，藉由光學顯微鏡進行觀察，於俯視接合構造體1時，分別劃定最大區域A0、中央區域A1及端部區域A2。之後，於通過最大區域A0之俯視時之圖心(相當於圖1(a)中第1被接合材11之俯視時之圖心)之位置，將樹脂包埋後之接合構造體沿厚度方向切斷，並對該切斷面進行研磨，進而藉由離子研磨對研磨面進行加工之後，例如如圖1(b)所示，製作與通過圖心之厚度方向剖面觀察相當之觀察面。
繼而，於上述觀察面中之中央區域A1內之任意位置，藉由使用電子顯微鏡進行目視觀察，以特定出作為測定對象之被接合材與接合部之界面G1或界面G2之位置。
繼而，於進行電子顯微鏡觀察時，例如藉由以測定視野之全長Lt為30 μm左右之方式拍攝複數張對象清晰之倍率之圖像並進行排列，而獲得全景圖像。於該狀態下，以被接合材11、12與接合部15之界面G1、G2中之一個界面為測定對象，測定該界面不清晰之部位之沿面方向X之長度La之合計，並將其作為中央區域A1之接合長度L1。替代地，接合長度L1可藉由自測定視野之全長Lt中減去作為測定對象之被接合材11、12與接合部15之界面G1、G2清晰之部位之合計長度而算出。接合長度L1可藉由以上述電子顯微鏡圖像或後述二值化圖像為對象，目視或根據需要使用軟體而算出。 於圖2(a)中，以第1被接合材11與接合部15之界面G1為例，示出了中央區域A1之全景圖像之模式圖。於該模式圖中，一併示出了全長Lt、長度La及接合長度L1。 並且，將中央區域之接合長度L1相對於測定視野之全長Lt之比(L1/Lt)作為本發明中之第1接合比率Rc。
同樣地，於上述觀察面上之端部區域A2內之任意位置，藉由使用電子顯微鏡進行目視觀察以特定出被接合材11、12與接合部15之界面G1、G2中之與用於測定接合比率Rc之界面相同之界面。
端部區域A2內之測定亦同樣，於電子顯微鏡觀察時，例如與上述方法同樣地以測定視野之全長Lt為30 μm左右之方式獲得全景圖像。於該狀態下，測定作為測定對象之被接合材11、12與接合部15之界面不清晰之部位之沿面方向X之長度Lb之合計，並將其作為端部區域A2之接合長度L2。替代地，接合長度L2可藉由自測定視野之全長Lt中減去各被接合材11、12與接合部15之界面清晰之部位之合計長度而算出。接合長度L2可藉由以上述電子顯微鏡圖像或後述二值化圖像為對象，目視或根據需要使用軟體而算出。 於圖2(b)中，以第1被接合材11與接合部15之界面G1為例，示出了端部區域A2之全景圖像之模式圖。於該模式圖中，一併示出了全長Lt、長度Lb及接合長度L2。 並且，將端部區域A2之接合長度L2相對於測定視野之全長Lt之比(L2/Lt)作為本發明中之接合比率Rs。
上述之「被接合材11、12與接合部15之界面G1、G2不清晰之部位」係指於製造接合構造體1時，金屬粒子與被接合材充分燒結之部位。另一方面，「被接合材11、12與接合部15之界面G1、G2清晰之部位」係指於製造接合構造體1時，金屬粒子與被接合材未燒結之部位。
被接合材11與接合部15之界面G1是否清晰係指於電子顯微圖像中，在作為測定對象之被接合材11與接合部15之界面G1處，沿厚度方向觀察二值化而得之二值化圖像時，若觀察到以相同顏色表示之區域與以不同顏色表示之區域之邊界，則被接合材11與接合部15之界面G1清晰。另一方面，若未觀察到上述邊界，則被接合材11與接合部15之界面G1不清晰。 針對被接合材12與接合部15之界面G2處，亦可與上述方法同樣地進行觀察，以判定界面G2為清晰還是不清晰。
再者，為了便於說明，關於接合比率Rc、Rs之測定方法，以接合構造體1之厚度方向上之一剖面視圖進行了說明，典型的是，接合構造體1中之各被接合材11、12與接合部15於最大區域A0之俯視全域中連續接合。因此，接合構造體1較佳為於考慮到以最大區域A0之俯視時之圖心為中心之虛擬圓、及通過該虛擬圓之中心且將該虛擬圓每隔30°切斷之虛擬放射狀線，觀察以該虛擬放射狀線每隔30°沿厚度方向切斷俯視時之接合構造體而得之剖面並測定出之各接合比率Rc、Rs均處於上述範圍內。
繼而，對接合構造體之製造方法進行說明。本製造方法大致分為如下3個步驟：塗佈步驟：其係於一個被接合材(例如被接合材12)之表面上塗佈包含銅之接合用組合物而形成塗膜；乾燥步驟：其係使該塗膜乾燥而形成乾燥塗膜；以及接合步驟：其係於該乾燥塗膜上進而積層另一個被接合材(例如被接合材11)，於該狀態下一面加壓一面加熱以使之接合。
首先，於一個被接合材之表面上塗佈包含銅之接合用組合物而形成塗膜(塗佈步驟)。接合用組合物較佳為含有包含銅之金屬粒子及液體介質者。接合用組合物之詳細內容於後文說明。
接合用組合物之塗佈方法較佳為採用可使所形成之塗膜之厚度均勻，並且可塗佈於預定塗佈面全域之方法。作為此種塗佈方法，例如可例舉網版印刷、分注印刷、凹版印刷、套版印刷等。就提高均勻塗佈性之觀點而言，接合用組合物較佳為包含液體介質之糊狀或油墨狀者。
關於所形成之塗膜之厚度，就形成穩定地具有高接合強度之接合構造體之觀點而言，於剛塗佈後，較佳為設定為1 μm以上250 μm以下，進而較佳為設定為5 μm以上150 μm以下。又，就於不產生被接合材與接合體相鄰而未密接之部分之狀態下，容易於被接合材與接合體之接合面全域中形成接合部，於接合面全域中提高與接合對象之接合強度之觀點而言，塗膜之俯視時之塗佈面積較佳為以作為接合對象之被接合材中之平面面積最小之被接合材之底面積以上之面積進行塗佈。
繼而，使所形成之塗膜乾燥而獲得乾燥塗膜(乾燥步驟)。於本步驟中，藉由乾燥自該塗膜中除去液體介質之至少一部分，而獲得塗膜中之液體介質之量減少之乾燥塗膜。藉由自塗膜中除去液體介質，可提高乾燥塗膜之保形性，又，於該狀態下將被接合材彼此接合，因此可提高接合強度。乾燥塗膜係指液體介質相對於膜之總質量之比率為9質量%以下者。塗膜及該塗膜乾燥後而成之乾燥塗膜之除液體介質以外之各構成材料之含量實質上相同，因此乾燥塗膜中之液體介質之比率例如可藉由測定乾燥前後之塗膜之質量變化而算出。
為了使液體介質乾燥並將其除去，可採用利用該液體介質之揮發性使液體介質揮發之方法，例如，可使用自然乾燥、熱風乾燥、紅外線照射、加熱板乾燥等乾燥方法。 除去液體介質後之乾燥塗膜中之該液體介質之比率相對於塗膜之總質量100質量份，較佳為如上所述為9質量份以下，進而較佳為7質量份以下，進而更佳為5質量份以下。 本步驟可根據所使用之接合用組合物之組成適當地變更，但就接合用組合物及與其一同進行乾燥之被接合材不易發生變質，維持被接合材之所需之物性，並可提高被接合材彼此之接合強度這一點而言，較佳為於大氣氛圍下，於40℃以上150℃以下、大氣壓下執行1分鐘以上60分鐘以下。
繼而，於乾燥塗膜上積層另一個被接合材進行接合(接合步驟)。詳細而言，經過上述步驟獲得乾燥塗膜後，將另一個被接合材積層至該乾燥塗膜上，而獲得在第1被接合材與第2之被接合材之間介置有乾燥塗膜而配置之積層體。該積層體例如為塗膜及第1被接合材以該順序積層於第2被接合材之一個面上者。 並且，對積層體一面進行加壓一面以規定之升溫速度進行加熱，以燒結乾燥塗膜中所包含之金屬粉，藉此形成將2個被接合材彼此接合之接合部。
燒結時之氣體氛圍較佳為氫或甲酸等還原氣體氛圍，或氮或氬等惰性氣體氛圍。 燒結溫度較佳為150℃以上350℃以下，更佳為200℃以上350℃以下，進而較佳為230℃以上300℃以下。
燒結時之升溫速度係於自40℃起升至上述燒結溫度為止之過程中，較佳為120℃/分鐘以上2000℃/分鐘以下，更佳為240℃/分鐘以上1500℃/分鐘以下，進而較佳為360℃/分鐘以上1000℃/分鐘以下。該升溫速度較製造先前之接合構造體時所採用之升溫速度快。藉由以上述速度進行升溫，可於短時間內製造出滿足上述Rs/Rc關係之接合構造體。
燒結時施加之壓力自加熱開始至燒結結束為止，較佳為維持在超過6 MPa且40 MPa以下，更佳為維持在8 MPa以上30 MPa以下，進而較佳為維持在10 MPa以上20 MPa以下。 燒結時間係以燒結溫度處於上述範圍內之狀態為條件，較佳為0.5分鐘以上120分鐘以下，更佳為1分鐘以上60分鐘以下，較佳為1分鐘以上30分鐘以下。
經過以上步驟，形成接合構造體1，該接合構造體1中，作為構成接合用組合物之包含銅之金屬粒子之燒結體之接合部15形成於2個被接合材11、12之間。根據上述之較佳之製造方法，可較佳地獲得在第1被接合材11與接合部15之間以及第2被接合材12與接合部15之間分別滿足上述Rs/Rc關係之接合構造體1。接合部15係包含銅者，又，於接合用組合物包含後述之固體還原劑之情形時，於接合層形成以下結構(1)。
[化1]
Figure 02_image001
式(1)中，R 3至R 5分別獨立地表示氫原子、羥基、碳原子數為1以上10以下之烴基或具有羥基之碳原子數為1以上10以下之烴基。R 3至R 5之詳細內容可適當應用後述化學式(2)及(3)之說明。又，＊表示與銅之鍵結部位。
關於接合層是否形成上述結構(1)，可藉由以接合部之剖面為對象，利用TOF-SIMS進行質量分析等來確認。例如，於使用BIS-TRIS作為還原劑之情形時，於TOF-SIMS之正極側之質譜中觀察到源於「C-N(Cu) 2」之m/z為152之碎片。
接合用組合物含有具有含銅之金屬粒子之金屬粉，較佳為進而含有還原劑及液體介質。
本發明中所使用之金屬粉較佳為含有含銅之金屬粒子之集合體。金屬粉可根據需要進而包含金、銀、鈀、鋁、鎳及錫中之至少一種金屬。
構成本發明所使用之金屬粉之金屬粒子之形狀例如為球狀、片狀、樹枝狀(dendrite狀)、棒狀等。其等可單獨使用或組合複數個而使用。
於金屬粒子為球狀之情形時之粒徑由藉由掃描式電子顯微鏡觀察之圖像解析而測定出之累積體積50容量%時之體積累積粒徑D SEM50表示，較佳為0.03 μm以上，更佳為0.05 μm以上。又，較佳為20 μm以下，更佳為10 μm以下。藉由形成為此種粒徑，可高生產性地形成薄型且具有均勻厚度之塗膜，可進而提高被接合材彼此之接合強度。
又，關於銅粒子為片狀之情形時之粒徑，利用雷射繞射散射式粒度分佈測定法而得之累積體積50容量%時之體積累積粒徑D 50較佳為0.3 μm以上，更佳為0.5 μm以上，進而較佳為0.7 μm以上。又，片狀之銅粒子之粒徑由D 50表示時，較佳為100 μm以下，更佳為70 μm以下，進而較佳為50 μm以下。藉由含有此種粒徑之粒子，可形成粒子彼此無間隙地配置之塗膜，可形成具有緻密構造之接合部，可表現出被接合材彼此之高接合強度。片狀係指具有形成粒子之主表面之一對板面及與該等板面正交之側面之形狀，板面及側面可分別獨立地為平面、曲面或凹凸面。
接合用組合物中所包含之還原劑較佳為於1氣壓、室溫(25℃)下為固體。此種還原劑用於促進藉由該組合物之焙燒而進行之金屬粒子彼此之燒結，從而表現出高接合強度。為了該目的，還原劑有利的為具有至少1個胺基及複數個羥基之化學結構者。「於室溫(25℃)下為固體」係指還原劑之熔點超過25℃。以下，亦將固體狀還原劑稱為「固體還原劑」。
固體還原劑之熔點較佳為金屬粉之燒結溫度以下。又，固體還原劑之沸點較佳為較後述液體介質之沸點高。藉由使用具有此種物性之固體還原劑，於使接合用組合物之塗膜乾燥而獲得乾燥塗膜時，可使固體還原劑以固體之形式殘留於接合用組合物中，其結果，可提高該接合用組合物之乾燥塗膜之保形性。
就有效率地表現出進行加壓接合時之高接合強度之觀點、及於使用導電體作為被接合材時，表現出加壓接合後之高導電可靠性之觀點而言，較佳為使用以下之化學式(2)或(3)表示之胺基醇化合物作為固體還原劑。
[化2]
Figure 02_image003
化學式(2)或(3)中，R 1至R 6分別獨立地表示氫原子、羥基、碳原子數為1以上10以下之烴基或具有羥基之碳原子數為1以上10以下之烴基。又，式(2)中，R 7表示碳原子數為1以上10以下之烴基或具有羥基之碳原子數為1以上10以下之烴基。作為烴基，可例舉飽和脂肪族基或不飽和脂肪族基。該脂肪族基可為直鏈狀者，或者亦可為支鏈狀者。
作為化學式(2)或(3)所表示之胺基醇化合物之具體例，可例舉：雙(2-羥乙基)亞胺基三(羥甲基)甲烷(BIS-TRIS，熔點為104℃，沸點超過300℃，對應於化學式(2))、2-胺基-2-(羥甲基)-1,3-丙二醇(TRIS，熔點為169～173℃，沸點超過300℃，對應於化學式(2))、1,3-二(三(羥甲基)甲胺基)丙烷(BIS-TRIS propane，熔點為164～165℃，沸點超過300℃，對應於化學式(3))等。其等之中，就獲得提高金屬粒子彼此之燒結性，並表現出高接合強度之接合體之觀點而言，較佳為使用雙(2-羥乙基)亞胺基三(羥甲基)甲烷作為固體還原劑。
上述固體還原劑可單獨使用一種，或者可組合二種以上使用。於任意情形下，就提高金屬粒子彼此之燒結性之觀點而言，接合用組合物中之固體還原劑之比率相對於100質量份之金屬粉較佳為0.1質量份以上，進而較佳為1質量份以上。又，就維持接合用組合物中金屬粉所占之比率，並發揮相對於被接合材之較佳塗佈性能之觀點而言，設為10質量份以下較現實，較佳為設為8質量份以下，進而較佳為設為5質量份以下。
就提高塗膜之塗佈性之觀點而言，接合用組合物較佳為進而包含液體介質。關於液體介質，就兼具接合用組合物之塗佈性、固體還原劑之溶解性以及伴隨液體介質之適度揮發性而提高乾燥塗膜之形成效率之觀點而言，較佳為非水溶劑，更佳為一元醇或多元醇，進而較佳為多元醇。
作為多元醇，例如可例舉：丙二醇、乙二醇、己二醇、二乙二醇、1,3-丁二醇、1,4-丁二醇、二丙二醇、三丙二醇、甘油、聚乙二醇200、聚乙二醇300等。液體介質可單獨使用一種或組合二種以上使用。
於接合用組合物中含有液體介質之情形下，就提高將接合用組合物塗佈於被接合材上時之塗膜之保形性及所形成之塗膜之厚度之均勻性之觀點而言，液體介質之含量相對於100質量份金屬粉，較佳為10質量份以上40質量份以下，進而較佳為10質量份以上35質量份以下。
只要能發揮本發明之效果，接合用組合物亦可包含其他成分，例如黏合劑成分、表面張力調整劑、消泡劑、黏度調整劑等。相對於100質量份金屬粉，其他成分之比率較佳為，總量為0.1質量份以上10質量份以下。
具有此種接合部之接合體可活用其高接合強度及導熱性之特性，而較佳地用於暴露於高溫之環境，例如車載電子線路及安裝有功率裝置之電子線路。 [實施例]
以下，藉由實施例進而對本發明進行詳細地說明。然而，本發明之範圍不限定於該等實施例。除非特別說明，否則「%」及「份」分別係指「質量%」及「質量份」。
〔實施例1〕 (1)接合用組合物之製備 使用D SEM50為0.14 μm之球狀銅粉與D 50為4.9 μm之長徑比(主表面之長度相對於粒子厚度之比)為13之片狀銅粉之混合物作為銅粉。球狀銅粉及片狀銅粉於銅粉之混合物中所占之含有比率設為，球狀銅粉70質量%：片狀銅粉30質量%。 以相對於100份之銅粉為2.5份之比率使用雙(2-羥乙基)亞胺基三(羥甲基)甲烷作為還原劑。 使用聚乙二醇300(相對於100份之銅粉為1份)與己二醇(相對於100份之銅粉為31.6份)之混合物作為液體介質。 將上述銅粉、還原劑及液體介質混合而獲得糊狀之接合用組合物。 剪切速度為10s -1時，接合用組合物之黏度於25℃時為34 Pa·s。
(2)接合構造體之製造 作為第2被接合材，於20 mm見方之俯視為正方形之銅板(厚度1 mm)之中央，藉由網版印刷塗佈接合用組合物而形成塗膜。塗膜使用厚度100 μm之金屬遮罩，於包括銅板之中央部之區域中形成為6 mm見方之正方形。使該塗膜於熱風乾燥機中以110℃乾燥10分鐘而除去一部分液體介質，置於室溫下，獲得乾燥塗膜。又，確認了乾燥塗膜中之液體介質之含量，結果為5質量%以下。
繼而，作為第1被接合材，將於表面全域中具有藉由Ag金屬化而形成之銀層的4.9 mm見方之俯視為正方形之半導體元件(SiC晶片，厚度0.38 mm，Wolfspeed公司製造，CPW5-1200-Z050B)載置於乾燥塗膜上，製成積層體。於該狀態下在厚度方向上施加20 MPa之壓力，於氮氣氛圍中，以960℃/分鐘之升溫速度自40℃起升溫至280℃，之後，在280℃下焙燒5分鐘，製作出具有圖1(a)及(b)所示之構造之接合構造體。該接合構造體之各被接合材及接合部於俯視之全域中相鄰地形成。又，藉由利用TOF-SIMS之質量分析確認了作為乾燥塗膜之燒結體之接合部形成有上述結構(1)所表示之化學結構。
〔實施例2〕 製造接合構造體時，將燒結時之施加壓力變更為10 MPa，除此以外，以與實施例1相同之方法，獲得具有圖1(a)及(b)所示之構造之接合構造體。藉由利用TOF-SIMS之質量分析確認了接合部形成有由上述結構(1)所表示之化學結構。
〔比較例1〕 製造接合構造體時，將燒結時之施加壓力變更為6 MPa，除此以外，以與實施例1相同之方法獲得接合構造體。藉由利用TOF-SIMS之質量分析確認了接合部形成有由上述結構(1)所表示之化學結構。
〔接合比率之測定〕 對於實施例及比較例之接合構造體，使用SYSTEMINFRONTIER股份有限公司製造之軟體MeasurementAdviser，用上述方法分別測定並計算被接合材與接合部之界面處之各接合比率Rc、Rs以及其等之比Rs/Rc。將其結果與測定視野之全長Lt一同示於以下之表1中。 再者，為了便於說明，於以下之表中，僅示出了SiC晶片(第1被接合材11)與接合部15之間之接合比率。
〔接合可靠性之評估〕 對於接合構造體，將冷熱循環試驗(TCT，thermal cycle test)進行10次循環，使用超音波探傷裝置(Hitachi Power Solutions Co.,Ltd.製造，型號為FineSAT III)，用75 MHz之探針利用反射法自銅板之背面側觀察此時自燒結體剝離之狀態。於TCT中，以(1)-40℃·15分鐘、(2)＋125℃·15分鐘為1個循環。 於觀察接合層之剝離狀態時，將增益值設為25～35dB之值之後，調節S閘門之延遲及寬度以使S閘門之峰值位置位於銅板之表面上。為了指定接合層之觀察範圍，調整了F閘門之延遲，並將寬度設定為1.5波長量之峰值寬度。調整探針之Z軸座標以使觀察峰值之振幅達到最大，並進行觀察。觀察圖像之對比度使用自動功能進行調節。 藉由上述裝置，接合狀態良好者觀察到顏色深(黑色)，發生龜裂或剝離而使接合狀態變差之區域觀察到顏色淺(白色)。其中，將實施例1及比較例1中之TCT前後之圖像資料示於圖3及圖4中。 又，使用圖像處理軟體Image-J對所獲得之圖像資料進行二值化，計算觀察到之面積中之黑色面積之比率(TCT進行10次循環後之接合率；%)。即，啟動Image-J後，選擇Analyze-Set measurement，並勾選Area、Area fraction、Limit to Threshold。之後，選擇File-Open，打開計算接合率之圖像資料之後，指定圖像中之SiC晶片搭載部之範圍(A)。繼而，選擇Edit-Copy to system，複製指定範圍(A)後，選擇File-New-System clipboard並黏貼指定範圍(A)之圖像。之後，為明確接合部，選擇Image-Type-8bit，轉換圖像後，選擇Image-Adjust-Threshold並將圖像之閾值調整至110。並且，指定調整後之圖像中之SiC晶片搭載部之範圍(A)內存在之紅色範圍(B)。上述紅色範圍(B)為SiC晶片接合部，其接合率可用(B)/(A)×100而算出。接合率越高，表示即使於發生過度之溫度變化之情形時接合可靠性亦越高。結果示於表1中。
[表1]
   實施例1 實施例2 比較例1
燒結溫度[℃] 280 280 280
燒結時間[分鐘] 5 5 5
升溫速度[℃/分鐘] 960 960 960
壓力[MPa] 20 10 6
接合 比率 中央區域A1 測定視野全長Lt[μm] 30.127 30.184 29.98
接合長度L1[μm] 19.554 14.711 6.812
接合比率Rc(L1/Lt) 0.65 0.49 0.23
端部區域A2 測定視野全長Lt[μm] 30.044 29.993 29.974
接合長度L2[μm] 15.165 10.756 8.852
接合比率Rs(L2/Lt) 0.50 0.36 0.30
Rs/Rc 0.78 0.74 1.30
接合可靠性之評估 TCT後之接合率[%] 97 97 20
[產業上之可利用性]
根據本發明，提供一種具有高接合可靠性之接合構造體。
1:接合構造體 11:被接合材 11e:被接合材11之周緣 12:被接合材 15:接合部 A0:最大區域 A1:中央區域 A2:端部區域 G1:被接合材11與接合部15之界面 G2:被接合材12與接合部15之界面 L1:接合長度 L2:接合長度 La:界面G1、G2中之一個界面不清晰之部位之沿面方向X之長度 Lb:被接合材11、12與接合部15之界面不清晰之部位之沿面方向X之長度 Lt:測定視野之全長 V1:虛擬區域 V2:虛擬區域 Z:厚度方向
圖1(a)係本發明之接合構造體之一實施方式之示意性俯視圖，圖1(b)係圖1(a)中之I-I線處之示意性剖視圖。 圖2(a)係示意性地示出於圖1(a)所示之接合構造體1之厚度方向上剖面觀察時，被接合材11與接合部15之界面之中央區域A1之全景圖像之放大圖，圖2(b)係示意性地示出於圖1(a)所示之接合構造體1之厚度方向上剖面觀察時，被接合材11與接合部15之界面之端部區域A2之全景圖像之放大圖。 圖3(a)係實施例1之接合構造體1之於冷熱循環試驗前之超音波圖像，圖3(b)係實施例1之接合構造體1之於冷熱循環試驗後之超音波圖像。 圖4(a)係比較例1之接合構造體1之於冷熱循環試驗前之超音波圖像，圖4(b)係比較例1之接合構造體1之於冷熱循環試驗後之超音波圖像。
1:接合構造體
11:被接合材
11e:被接合材11之周緣
12:被接合材
15:接合部
A0:最大區域
A1:中央區域
A2:端部區域
G1:被接合材11與接合部15之界面
G2:被接合材12與接合部15之界面
V1:虛擬區域
V2:虛擬區域
Z:厚度方向

Claims (3)

  1. 一種接合構造體，其係由2個被接合材及相鄰地形成於該等被接合材之間之接合部接合而成者， 上述接合部由以銅為主體之材料構成， 於上述接合構造體之厚度方向剖面觀察時，該接合構造體之端部區域中之上述被接合材與上述接合部之接合比率Rs相對於該接合構造體之中央區域中之上述被接合材與上述接合部之接合比率Rc之比(Rs/Rc)為0.6以上0.9以下，且 上述接合比率Rc為0.3以上。
  2. 如請求項1之接合構造體，其中上述被接合材中之至少一者之表面具有金、銀、銅、鎳以及鈦中之至少一種金屬。
  3. 如請求項1之接合構造體，其中於上述接合部形成下式(1)所示之結構： [化1]
    Figure 03_image005
    (式(1)中，R 3至R 5分別獨立地表示氫原子、羥基、碳原子數為1以上10以下之烴基或具有羥基之碳原子數為1以上10以下之烴基， ＊表示與銅之鍵結部位)。
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