TW202204482A - 積層體、硬化性樹脂組成物、積層體之製造方法、具有接合電極之基板的製造方法、半導體裝置及攝影裝置 - Google Patents

積層體、硬化性樹脂組成物、積層體之製造方法、具有接合電極之基板的製造方法、半導體裝置及攝影裝置 Download PDF

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TW202204482A
TW202204482A TW110122578A TW110122578A TW202204482A TW 202204482 A TW202204482 A TW 202204482A TW 110122578 A TW110122578 A TW 110122578A TW 110122578 A TW110122578 A TW 110122578A TW 202204482 A TW202204482 A TW 202204482A
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substrate
laminate
organic film
curable resin
resin composition
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TW110122578A
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塩島太郎
佐藤憲一朗
出口英寛
石澤英亮
畠井宗宏
七里徳重
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日商積水化學工業股份有限公司
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Abstract

本發明之目的在於提供一種具有高電連接可靠性之積層體、用於該積層體之硬化性樹脂組成物、該積層體之製造方法、用於製造該積層體之具有接合電極之基板的製造方法、及具有該積層體之半導體裝置及攝影裝置。本發明係一種積層體，其依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，上述第1基板所具有之電極與上述第2基板所具有之電極經由貫通上述有機膜之貫通孔而電連接。

Description

積層體、硬化性樹脂組成物、積層體之製造方法、具有接合電極之基板的製造方法、半導體裝置及攝影裝置
本發明係關於一種具有高電連接可靠性之積層體、用於該積層體之硬化性樹脂組成物、該積層體之製造方法、用於製造該積層體之具有接合電極之基板的製造方法、及具有該積層體之半導體裝置及攝影裝置。
隨著半導體裝置之高性能化，將複數個半導體晶片進行積層之三維化正不斷發展。於此種積層有複數個半導體晶片之積層體之製造中，首先，藉由金屬鑲嵌法，於2片形成有電極之基板之電極面，形成由銅構成之接合電極被絕緣膜包圍之接合面。之後，以接合面之接合電極彼此對向之方式將2片基板重疊，並實施熱處理，藉此製造積層體（專利文獻1）。 先前技術文獻 專利文獻
專利文獻1：日本特開2006-191081號公報
[發明所欲解決之課題]
於上述積層體之製造中，在將電極接合時，會實施400℃、4小時之高溫處理，因此對用於形成上述接合面之絕緣膜要求較高之耐熱性。因此，於以往之積層體中，使用SiN或SiO2 等絕緣性無機材料作為絕緣體。然而，由無機材料構成之絕緣膜存在如下問題，即，基板容易產生翹曲，若基板產生翹曲，則製成積層體時，電極之連接位置會發生偏移，或者電極會發生破裂，因此積層體之連接可靠性有時會降低。又，近年來，半導體裝置之高性能化不斷發展，基板逐漸大型化、薄化，使得基板更容易產生翹曲。
本發明之目的在於提供一種具有高電連接可靠性之積層體、用於該積層體之硬化性樹脂組成物、該積層體之製造方法、用於製造該積層體之具有接合電極之基板的製造方法、及具有該積層體之半導體裝置及攝影裝置。 [解決課題之技術手段]
本發明係一種積層體，其依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，且上述第1基板所具有之電極與上述第2基板所具有之電極經由貫通上述有機膜之貫通孔而電連接。以下，對本發明加以詳細敍述。
本發明之積層體依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，且上述第1基板所具有之電極（第1電極）與第2基板所具有之電極（第2電極）經由貫通上述有機膜之貫通孔而電連接。 設置於第1電極與第2電極之間之有機膜發揮絕緣層之作用，藉此可抑制電流之短路。以往之絕緣層係使用SiN或SiO2 等堅固之無機材料，因此若於形成絕緣層時或形成積層體時產生翹曲，無法藉由應力緩和來消除該翹曲，結果容易引起電極之偏移或破裂。於本發明中，藉由使用柔軟性高於無機材料之有機膜作為絕緣層，可發揮較高之電連接可靠性。尤其是，即便於基板或積層體產生翹曲之情形時，亦可消除翹曲，因此，即便積層容易產生翹曲之較薄基板時，電極之偏移或破裂亦較少，能夠製成具有高電連接可靠性之積層體。又，以往之絕緣層係藉由蒸鍍而形成，因此其形成要耗費時間，但本發明之積層體之有機膜例如可藉由硬化性樹脂之塗佈、硬化而形成，因此可提高生產效率。 再者，此處所謂電連接，係指第1基板之電極與第2基板之電極藉由填充於上述貫通孔中之導電性材料等而連接的狀態。
上述第1基板及第2基板並無特別限定，可使用形成有元件、配線及電極之電路基板。例如，可使用設置有像素部（像素區域）之感測器電路基板、搭載有執行與固體攝影裝置之動作相關的各種訊號處理之邏輯電路等周邊電路部之電路基板等。
上述第1基板及第2基板所具有之電極之材料及上述導電性材料並無特別限定，可使用金、銅、鋁等先前公知之電極材料。
上述有機膜只要是含有有機化合物作為素材之層則並無特別限定，較佳為含有樹脂作為素材之層。上述有機膜亦可於不明顯損害本發明之效果之範圍內含有上述樹脂素材以外之成分。於此情形時，有機膜中之樹脂素材之含量例如較佳為90重量%以上，更佳為95重量%以上，進而較佳為99重量%以上，通常未達100重量%。 作為上述樹脂素材，可使用下述有機矽化合物、聚矽氧烷樹脂等。
較佳為上述有機膜於進行400℃、4小時之熱處理後，重量損失率為5%以下。 藉由使有機膜之熱處理後之重量損失率處於上述範圍內，可更確實地將基板接合，並且可進一步抑制因電極接合時分解之有機膜而引起界面處之氣泡、龜裂之產生或界面處之剝離。上述重量損失率更佳為3%以下，進而較佳為1%以下。上述重量損失率之下限並無特別限定，越接近0%越佳，但製造技術上之極限為0.5%左右。 上述400℃、4小時之熱處理後之重量損失率可根據有機膜之組成、構成有機膜之樹脂素材之種類、製造有機膜時之硬化條件等來進行調整。 具體而言，例如藉由使用譬如耐熱性較高之樹脂素材或無機成分作為有機膜之組成、增加交聯劑之含量等，可降低上述400℃、4小時之熱處理後之重量損失率。 又，藉由將構成有機膜之樹脂素材之種類設為耐熱性較高之樹脂（例如，分子量較大之樹脂或具有耐熱性較高之主鏈或取代基之樹脂、下述有機矽化合物），或者將構成有機膜之硬化性樹脂組成物之硬化條件設為如使硬化充分進行之高溫，或將硬化時間設為較長時間，可降低上述400℃、4小時之熱處理後之重量損失率。
較佳為上述有機膜之藉由奈米壓痕儀測得之表面硬度為5 GPa以下。 由於表面硬度處於上述範圍內之有機膜之柔軟性較高，故基板或積層體更加不容易產生翹曲，又，即便產生翹曲，亦更容易將其消除，因此可進一步抑制電極之偏移或破裂。 上述表面硬度更佳為5 GPa以下，進而較佳為1 GPa以下。 上述表面硬度之下限並無特別限定，例如為0.1 GPa、0.2 GPa，較佳為0.3 GPa。 上述有機膜之藉由奈米壓痕儀測得之表面硬度可根據構成上述有機膜之樹脂成分之種類或有機膜之組成來進行調整。具體而言，例如可藉由導入玻璃轉移點較高之剛直骨架或添加無機填充劑來提高表面硬度，可藉由使用具有玻璃轉移點較低之剛直骨架的化合物或下述有機矽化合物來降低表面硬度。 再者，此處所謂奈米壓痕儀，係指根據向試樣表面刺入針時所施加之力與應力之關係來測定硬度之裝置，可測定試樣之硬度。上述表面硬度例如可利用以下方法進行測定。 首先，利用冷樹脂包埋積層體之側面（積層面），並藉由剖面研削裝置對其進行研削，直至有機膜露出。之後，使用奈米壓痕儀（TI 950 TriboIndenter，Scienta Omicron公司製造或其同等品），於以下條件下進行測定，藉此可獲得上述表面硬度：於測定溫度23℃，以測定位移200 nm/秒之速度將樣品壓入1000 nm，之後以200 nm/秒之速度拔出測定探針。再者，測定探針使用Berkovich型金剛石壓頭。
上述有機膜之厚度並無特別限定，較佳為10 μm以上300 μm以下。 藉由使有機膜之厚度處於上述範圍內，可更好地發揮其作為絕緣層之功能，並且可進一步抑制電極之偏移或破裂。上述有機膜之厚度更佳為20 μm以上，進而較佳為30 μm以上，更佳為200 μm以下，進而較佳為100 μm以下。
上述有機膜較佳為含有有機矽化合物，較佳為具有下述通式（1）所表示之結構。藉由使用有機矽化合物，可進一步抑制電極之偏移或破裂。又，由於有機矽化合物之耐熱性優異，故可進一步抑制因製造積層體時或製造使用積層體之電子零件時所進行之高溫處理而導致有機膜分解。其中，就進一步提高耐熱性且進一步抑制電極之偏移或破裂之方面而言，上述有機矽化合物更佳為進而具有芳香環結構。
Figure 02_image001
此處，R0 、R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。m、n分別表示1以上之整數。
上述通式（1）中R0 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。上述R0 較佳為苯基、碳數1～20之烷基或芳烷基，更佳為苯基。藉由使R0 為苯基、碳數1～20之烷基或芳烷基，可發揮更高之耐熱性。
上述通式（1）中R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。上述R1 及R2 較佳為苯基、碳數1～20之烷基或芳烷基，更佳為苯基或甲基。藉由使R1 及R2 為苯基、碳數1～20之烷基或芳烷基，可發揮更高之耐熱性。
上述通式（1）中，m、n分別為1以上之整數，表示重複單元數。上述m較佳為30以上，更佳為50以上，較佳為100以下。上述n較佳為1以上，更佳為3以上，較佳為8以下。
上述有機膜較佳為硬化性樹脂組成物之硬化物。 藉由使用硬化性樹脂組成物作為上述有機膜之材料，可在塗佈硬化性樹脂組成物進行成膜後，使其硬化從而形成有機膜，因此相較於使用以往之無機材料之情形，可提高生產效率。構成硬化性樹脂組成物之硬化性樹脂可為熱硬化性，亦可為光硬化性，就耐熱性之觀點而言，較佳為熱硬化性樹脂。
上述硬化性樹脂組成物較佳為含有具有反應性部位之有機矽化合物。 藉由使用具有反應性部位之有機矽化合物作為硬化性樹脂組成物之硬化性樹脂，可進一步抑制電極之偏移或破裂。又，由於有機矽化合物之耐熱性優異，故可進一步抑制因製造積層體或製造使用積層體之電子零件時所進行之高溫處理而導致有機膜分解。作為上述反應性部位，例如可列舉羥基、烷氧基等。
於上述硬化性樹脂組成物中之樹脂固形物成分量100重量份中，上述具有反應性部位之有機矽化合物之含量較佳為80重量份以上，更佳為90重量以上，進而較佳為95重量份以上。於上述硬化性樹脂組成物中之樹脂固形物成分量100重量份中，上述具有反應性部位之有機矽化合物之含量較佳為未達100重量份，更佳為98重量份以下。
上述具有反應性部位之有機矽化合物較佳為具有下述通式（1）所表示之結構。 藉由使用此種具有反應性部位之有機矽化合物，可進一步抑制電極之偏移或破裂。其中，就可進一步抑制電極之偏移或破裂之方面而言，上述具有反應性部位之有機矽化合物更佳為具有芳香環結構。
Figure 02_image001
此處，R0 、R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。m、n分別表示1以上之整數。
上述通式（1）中R0 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。上述R0 較佳為苯基、碳數1～20之烷基或芳烷基，更佳為苯基。藉由使R0 為苯基、碳數1～20之烷基或芳烷基，可發揮更高之耐熱性。
上述通式（1）中R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫。上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基。上述R1 及R2 較佳為苯基、碳數1～20之烷基或芳烷基，更佳為苯基或甲基。藉由使R1 及R2 為苯基、碳數1～20之烷基或芳烷基，可發揮更高之耐熱性。
上述通式（1）中，m、n分別為1以上之整數，表示重複單元數。上述m較佳為30以上，更佳為50以上，較佳為100以下。上述n較佳為1以上，更佳為3以上，較佳為8以下。
上述硬化性樹脂組成物之硬化物於25℃之拉伸彈性模數較佳為5 GPa以下。藉由使拉伸彈性模數處於上述範圍內，可進一步提高柔軟性，因此可進一步抑制基板及積層體產生翹曲，可進一步抑制電極之偏移或破裂。上述拉伸彈性模數更佳為1 GPa以下，進而較佳為700 MPa以下，進而更佳為500 MPa以下。上述拉伸彈性模數之下限並無特別限定，就確實地連接基板彼此之觀點而言，較佳為100 MPa以上。再者，上述拉伸彈性模數可利用動態黏彈性測定裝置（例如，日本IT計測控制公司（ITKDVA）製造，DVA-200等）進行測定。更具體而言，於硬化性樹脂組成物為熱硬化性之情形時，以70℃加熱30分鐘後，進而以90℃加熱1小時，藉此進行溶劑乾燥，進而以200℃加熱1小時而使硬化性樹脂組成物硬化，然後於定速升溫拉伸模式、升溫速度10℃/分鐘、頻率10 Hz之條件下進行測定。於硬化性樹脂組成物為光硬化性之情形時，可以70℃加熱30分鐘後，進而以90℃加熱1小時，藉此進行溶劑乾燥，並以3000 mJ/cm2 照射405 nm之UV而使硬化性樹脂組成物硬化，之後，在與熱硬化性之硬化性樹脂組成物同樣之測定條件下進行測定。 上述於25℃之拉伸彈性模數可根據硬化性樹脂組成物之組成或硬化性樹脂之種類進行調整。 具體而言，例如可藉由導入玻璃轉移點較高之剛直骨架或添加無機填充劑來提高拉伸彈性模數，可藉由使用具有玻璃轉移點較低之剛直骨架的化合物或上述有機矽化合物來降低拉伸彈性模數。
上述硬化性樹脂之重量平均分子量並無特別限定，較佳為5000以上150000以下。藉由使硬化性樹脂之分子量處於上述範圍內，能夠提高塗佈時之製膜性，並進一步抑制電極之偏移或破裂。上述硬化性樹脂之分子量更佳為10000以上，進而較佳為30000以上，更佳為100000以下，進而較佳為70000以下。 再者，上述硬化性樹脂之重量平均分子量係藉由凝膠滲透層析（GPC）法，以聚苯乙烯換算分子量之形式測得。可以THF為溶析溶劑，使用HR-MB-M6.0×150 mm（Waters公司製造）或其同等品作為管柱，根據聚苯乙烯標準，來算出上述硬化性樹脂之重量平均分子量。
關於具有上述通式（1）之結構之化合物，例如可藉由使下述通式（2）所表示之化合物（2）與下述通式（3）所表示之化合物（3）反應而獲得。
Figure 02_image004
上述通式（2）中，R0 及R1 表示與上述通式（1）中之R0 及R1 相同之官能基。
Figure 02_image006
上述通式（3）中，R2 表示與上述通式（1）中之R2 相同之官能基。上述通式（3）中，h表示自然數，較佳為3～6，更佳為3或4。
具有上述通式（1）之結構之化合物亦可藉由使具有R2 之鹵化矽氧烷（例如末端經氯化之二甲基矽氧烷等）代替上述化合物（3）來與上述化合物（2）反應而獲得。
上述化合物（2）例如可藉由使下述通式（4）所表示之化合物（4）之類的鹽與下述通式（5）所表示之化合物（5）反應而獲得。再者，上述化合物（2）亦可藉由使用X為氫之化合物（5）來與化合物（4）反應後進行水解而獲得。
Figure 02_image008
上述通式（4）中，R0 表示與上述通式（1）中之R0 相同之官能基。
Figure 02_image010
上述通式（5）中，R1 表示與上述通式（1）中之R1 相同之官能基，X表示氫或羥基。
上述化合物（4）例如可藉由如下方法加以製造，即，於存在一價鹼金屬氫氧化物及水之情況下，於存在或不存在有機溶劑之情況下，使下述通式（6）所表示之化合物（6）進行水解、縮聚。作為一價鹼金屬氫氧化物，可使用：氫氧化鋰、氫氧化鈉、氫氧化鉀、氫氧化銫等。
Figure 02_image012
上述通式（6）中，R0 表示與上述通式（1）中之R0 相同之官能基。
上述硬化性樹脂組成物較佳為含有促進硬化反應之觸媒。 藉由使硬化性樹脂組成物含有觸媒，可使硬化性樹脂更完全地硬化，可進一步抑制因高溫處理而導致有機膜分解。 作為上述觸媒，例如可列舉：二月桂酸二丁基錫、乙酸亞錫等有機錫化合物；環烷酸鋅等金屬羧酸鹽；氧化鋯化合物；鈦化合物等。其中，就可進一步促進硬化性樹脂組成物之硬化之方面而言，較佳為二月桂酸二丁基錫。 上述觸媒於硬化性樹脂組成物硬化後仍存在。即，上述有機膜較佳為含有促進硬化反應之觸媒。
上述觸媒之含量並無特別限定，相對於上述硬化性樹脂組成物中之硬化性樹脂100重量份，較佳為0.01重量份以上10重量份以下。藉由將觸媒之含量設為上述範圍，可進一步促進硬化性樹脂組成物之硬化。上述觸媒之含量更佳為0.1重量份以上，進而較佳為1重量份以上，更佳為7重量份以下，進而較佳為5重量份以下。
上述硬化性樹脂組成物較佳為含有多官能交聯劑，該多官能交聯劑可與上述具有反應性部位之有機矽化合物之反應性部位發生反應。 可與有機矽化合物之反應性部位發生反應的多官能交聯劑會使上述具有反應性部位之有機矽化合物之聚合物間相交聯，藉此提高硬化物之交聯密度，進一步抑制高溫中之分解。其結果，可進一步抑制因高溫處理中產生分解氣體而導致產生空隙、或由此導致連接時電極偏移或電連接可靠性降低。作為上述多官能交聯劑，例如，於上述反應性部位為矽烷醇基之情形時，可列舉：二甲氧基矽烷化合物、三甲氧基矽烷化合物、二乙氧基矽烷化合物、三乙氧基矽烷化合物等烷氧基矽烷化合物等；或藉由四甲氧基矽烷化合物及四乙氧基矽烷化合物之縮合而獲得之矽酸酯低聚物等。其中，就提高交聯密度及提高耐熱性之觀點而言，較佳為矽酸酯低聚物。作為烷氧基矽烷化合物之例，有二甲氧基二甲基矽烷、三甲氧基甲基矽烷、四乙氧基矽烷、四丙氧基矽烷、四丁氧基矽烷等，作為矽酸酯低聚物之例，可列舉：矽酸酯MS51、MS56、MS57、MS56S（均由Mitsubishi Chemical公司製造）、矽酸乙酯40、矽酸乙酯48、EMS485（均由COLCOAT公司製造）等。
上述多官能交聯劑之含量並無特別限定，相對於上述硬化性樹脂組成物中之硬化性樹脂100重量份，較佳為1重量份以上50重量份以下。藉由將多官能交聯劑之含量設為上述範圍，可使有機膜之交聯密度處於適當範圍內，並且使熱處理時之有機膜之硬度處於上述範圍內。上述多官能交聯劑之含量更佳為3重量份以上，進而較佳為5重量份以上，更佳為30重量份以下，進而較佳為20重量份以下。
上述硬化性樹脂組成物亦可視需要含有黏度調整劑、填充劑、密接賦予劑等其他添加劑。
本發明之積層體藉由使上述硬化性樹脂組成物硬化來製成上述有機膜，而能夠製成具有高電連接可靠性之積層體。 此種用於積層體之上述有機膜之硬化性樹脂組成物亦為本發明之一，上述積層體依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，且上述第1基板所具有之電極與第2基板所具有之電極經由貫通上述有機膜之貫通孔而電連接。
本發明之積層體較佳為於上述第1基板與上述第2基板之間具有厚度1 nm以上1 μm以下之無機層。 藉由在第1基板與第2基板之間設置無機層，可製成絕緣性提高且連接可靠性更優異之積層體。再者，先前由於具有厚10～20 μm左右之由無機材料構成之絕緣層，故無法消除基板及積層體之翹曲而導致連接可靠性降低，但本發明之一形態之無機層具有1 μm以下之較薄厚度，因此即便於設置上述無機層之情形時，亦可消除基板及積層體所產生之翹曲。
上述無機層之材料並無特別限定，例如可列舉SiN、SiO2 、Al2 O3 等。其中，就絕緣性及耐熱性優異之方面而言，較佳為SiN、SiO2 。
就進一步提高積層體之連接可靠性之觀點而言，上述無機層之厚度更佳為5 nm以上，進而較佳為10 nm以上，更佳為500 nm以下，進而較佳為100 nm以下。
本發明之積層體較佳為於上述貫通孔之表面具有障壁金屬層。 障壁金屬層具有防止貫通孔中填充之導電性材料（例如於Cu電極之情形時為Cu原子）擴散至有機膜中之作用。藉由在貫通孔之表面設置障壁金屬層，貫通孔中填充之導電性材料除與電極相接之面以外均被障壁金屬層覆蓋，因此可進一步抑制導電性材料擴散至有機膜而導致短路、導通不良。上述障壁金屬層之材料可使用鉭、氮化鉭、氮化鈦等公知之材料。
上述障壁金屬層之厚度並無特別限定，就進一步提高積層體之連接可靠性之觀點而言，更佳為1 nm以上，進而較佳為10 nm以上，更佳為100 nm以下，進而較佳為50 nm以下。
此處，於圖1中示出示意性地表示本發明之積層體之一態樣之圖。如圖1所示，本發明之積層體為如下構造：具有電極3之第1基板1及第2基板2經由有機膜4而接著，第1基板1及第2基板2上之電極3通過設置於有機膜4上之貫通孔5中填充的導電性材料而電連接。以往之積層體由於充當絕緣層之有機膜4之部分為堅固之無機材料，故於基板或積層體產生翹曲之情形時，無法藉由應力緩和來消除該翹曲，而容易發生電極之偏移或破裂。本發明藉由將具有柔軟性之有機化合物用於絕緣層，而可消除基板或積層體之翹曲，因此可抑制電極之偏移或破裂。
於圖2中示出示意性地表示本發明之積層體之一態樣的圖。於圖2之態樣中，於有機膜4之間設置有無機層6，可進一步提高絕緣性。再者，由於本發明之無機層6之厚度為1 nm～1 μm，薄於以往之積層體之絕緣層，故於消除基板或積層體之翹曲時，不會產生妨礙。又，於圖2中，無機層6設置於有機膜4之間，但亦可設置於第1基板1及第2基板2上。又，於圖2中，無機層6分別設置於第1基板1側及第2基板2側之有機膜4上，但亦可僅設置於其中一者上。進而，於圖2之態樣中，於貫通孔5之表面設置有障壁金屬層7。藉由在貫通孔5之表面形成障壁金屬層7，貫通孔5內填充之導電性材料不易擴散至有機膜4，故可進一步抑制短路或導通不良。
作為製造本發明之積層體之方法，例如可列舉包括以下步驟之製造方法：於具有電極之第1基板的電極形成面上形成有機膜之步驟；於上述有機膜上形成貫通孔之步驟；用導電性材料填充上述貫通孔之步驟；對上述基板之填充有導電性材料之側之表面進行研磨，而形成接合電極之步驟；以及以上述接合電極彼此接合之方式，將形成有上述接合電極之上述第1基板與形成有上述接合電極之第2基板貼合之步驟。此種積層體之製造方法亦為本發明之一。
關於本發明之積層體之製造方法，首先實施於具有電極之第1基板的電極形成面上形成有機膜之步驟。 上述具有電極之第1基板、第2基板及有機膜可使用與本發明之積層體之具有電極之第1基板、第2基板及有機膜相同者。
形成上述有機膜之步驟較佳為除塗佈硬化性樹脂組成物後進行溶劑乾燥以外，還具有使硬化性樹脂組成物硬化之步驟。 上述硬化性樹脂組成物可使用與本發明之硬化性樹脂組成物相同者。 上述塗佈之方法並無特別限定，可使用旋轉塗佈法等先前公知之方法。 溶劑乾燥條件並無特別限定，就減少殘留溶劑、提高有機膜之耐熱性之觀點而言，宜於較佳為70℃以上、更佳為100℃以上、較佳為250℃以下、更佳為200℃以下之溫度，加熱例如30分鐘、更佳為1小時左右。 硬化條件並無特別限定，就使硬化反應充分進行、使耐熱性進一步提高之觀點而言，於硬化性樹脂組成物為熱硬化性樹脂之情形時，宜於較佳為200℃以上、更佳為220℃以上、較佳為400℃以下、更佳為300℃以下之溫度，加熱例如1小時以上、更佳為約2小時以上。加熱時間之上限並無特別限定，就抑制有機膜之熱分解之觀點而言，較佳為3小時以下。於硬化性樹脂組成物為光硬化性樹脂之情形時，宜將405 nm之紫外光照射較佳為1500 mJ/cm2 以上、更佳為3000 mJ/cm2 以上。
關於本發明之積層體之製造方法，繼而實施於上述有機膜形成貫通孔之步驟。 上述貫通孔可經圖案化。形成上述貫通孔之方法並無特別限定，可藉由CO2 雷射等雷射照射或蝕刻等而形成。再者，於基板之電極面上形成有其他層時，上述貫通孔以亦貫通上述其他層而使基板之電極面露出之方式形成。
關於本發明之積層體之製造方法，繼而視需要實施形成無機層及/或障壁金屬層之步驟。 上述無機層及障壁金屬層可使用與本發明之積層體相同者。上述無機層及障壁金屬層可藉由濺鍍或蒸鍍等而形成。 形成上述無機層之步驟較佳為於形成上述有機膜之步驟之前及/或之後實施。上述障壁金屬層之形成較佳為於形成上述貫通孔之步驟之後實施。
關於本發明之積層體之製造方法，繼而實施用導電性材料填充上述貫通孔之步驟。作為填充上述導電性材料之方法，可使用鍍覆等。 上述導電性材料可使用與本發明之積層體之導電性材料相同者。
關於本發明之積層體之製造方法，繼而實施對上述基板之填充有導電性材料之側之表面進行研磨而形成接合電極的步驟。 藉由利用研削去除形成於無用部分之上述導電性材料，而形成將2片基板上形成之電極間連接之接合電極。上述研磨較佳為平坦化去除由導電性材料形成之層，直至有機膜露出，或於存在上述無機層之情形時，直至無機層露出。 上述研磨方法並無特別限定，例如可使用化學機械研磨法等。
此種具有接合電極之基板的製造方法亦為本發明之一，該製造方法包括以下步驟：於具有電極之基板的電極形成面上形成有機膜之步驟；於上述有機膜形成貫通孔之步驟；用導電性材料填充上述貫通孔之步驟；及對上述基板之表面進行研磨而形成接合電極之步驟。 上述具有接合電極之基板係用於藉由以基板間之接合電極彼此接合之方式貼合而形成積層體的構件。關於上述基板、有機膜、硬化性樹脂組成物及其他構成及各步驟，與本發明之積層體、硬化性樹脂組成物及積層體之製造方法之相關說明相同。
關於本發明之積層體之製造方法，繼而實施以上述接合電極彼此接合之方式，將形成有上述接合電極之上述第1基板與形成有上述接合電極之第2基板貼合的步驟。 作為將第1基板與第2基板貼合之方法，可列舉藉由熱處理使接合電極熔融而進行連接之方法等。上述熱處理通常為400℃、4小時左右。
本發明之積層體之用途並無特別限定，就具有高電連接可靠性，尤其是使薄基板彼此接合時亦可抑制基板或積層體之翹曲之方面而言，適宜用於構成半導體裝置、攝影裝置之積層體。 此種具有本發明之積層體之半導體裝置及攝影裝置亦為本發明之一。 [發明之效果]
根據本發明，可提供一種具有高電連接可靠性之積層體、用於該積層體之硬化性樹脂組成物、該積層體之製造方法、用於製造該積層體之具有接合電極之基板的製造方法、及具有該積層體之半導體裝置及攝影裝置。
以下舉出實施例來更詳細地說明本發明之態樣，但本發明並不僅限定於該等實施例。
（硬化性樹脂之製造） （1）POSS-A之製造 向安裝有回流冷凝器、溫度計、及滴液漏斗之反應容器中，加入苯基三甲氧基矽烷（東京化成工業公司製造，分子量198.29）320 g、氫氧化鈉8.8 g、水6.6 g、及2-丙醇263 mL。於氮氣氣流下，一面攪拌一面開始加熱。回流開始後繼續攪拌6小時，然後於室溫靜置1夜。然後將反應混合物轉移至過濾器，利用氮氣進行加壓過濾。利用2-丙醇對所獲得之固體進行1次清洗，並進行過濾，然後於80℃進行減壓乾燥，藉此獲得無色固體（DD-ONa）330 g。
繼而，向安裝有回流冷凝器、溫度計、及滴液漏斗之反應容器中加入環戊基甲醚20 g、2-丙醇2.4 g、離子交換水14 g、二氯甲基矽烷（東京化成工業公司製造，分子量115.03）7.25 g，於氮氣環境下，於室溫進行攪拌。繼而，向滴液漏斗中加入上述獲得之化合物（DD-ONa）8 g、環戊基甲醚20 g，形成漿料狀，並歷時30分鐘滴加至反應器中，滴加結束後，繼續攪拌30分鐘。反應後停止攪拌，進行靜置而分為有機層及水層。藉由水洗將所獲得之有機層調整為中性後，利用膜濾器去除雜質，使用旋轉蒸發器於60℃進行減壓濃縮，獲得9.5 g之無色固體。利用乙酸甲酯10 g對該無色固體進行清洗，並進行減壓乾燥，而獲得無色粉末狀之固體（DD（Me）-OH）6.2 g。
於100 mL之燒瓶上安裝冷凝管、機械攪拌器、迪安-斯塔克管、油浴槽、溫度計保護管，並對燒瓶內部進行氮氣置換。將5.0 g之DD（Me）-OH、2.5 g之八甲基環四矽氧烷（D4）、0.5 g之RCP-160M（強酸性陽離子交換樹脂，三菱化學（股）製造，含水量23.4質量%）、51.0 mL之脫水甲苯添加至燒瓶中。進行1小時回流，取出甲苯22.4 mL及RCP-160M中以23.4質量%包含之水0.12 g。回流結束後，冷卻至80℃，並加入純水0.55 g，於80℃使其熟化，5小時後達到平衡。冷卻至室溫後，對RCP-160M進行過濾，對所獲得之濾液進行1次水洗。之後，將濾液之溶劑及低沸成分蒸餾去除，利用庚烷使所獲得之粗產物再沈澱而進行純化，藉此獲得具有下述式（7）之結構且m2為55、n2平均為4之有機矽化合物（POSS-A，重量平均分子量13萬）。
Figure 02_image014
（2）POSS-B之製造 除將八甲基環四矽氧烷之投入量設為5.0 g以外，藉由與POSS-A之製造相同之方法獲得具有上述式（2）之結構且m2為38、n2平均為8之有機矽化合物（POSS-B，重量平均分子量13萬）。
（3）POSS-C之製造 除將八甲基環四矽氧烷之投入量設為1.5 g以外，藉由與POSS-A之製造相同之方法獲得具有上述式（2）之結構且m2為50、n2平均為2之有機矽化合物（POSS-C，重量平均分子量9萬）。
（4）POSS-D之製造 將苯基三甲氧基矽烷變更為甲基三甲氧基矽烷（東京化成工業公司製造，分子量136.22），並將投入量設為210 g，除此以外，藉由與POSS-A之製造相同之方法獲得具有下述式（8）之結構且m2為60、n2平均為4之有機矽化合物（POSS-D，重量平均分子量11萬）。
Figure 02_image016
（5）POSS-E 使用小西化學工業公司製造之SR-13。再者，SR-13係不滿足式（1）之矽倍半氧烷（silsesquioxane）化合物。
（6）POSS-F 使用小西化學工業公司製造之SR-33。再者，SR-33係具有芳香環基且不滿足式（1）之矽倍半氧烷。
（7）PDMS樹脂 使用信越化學公司製造之KR-255作為PDMS樹脂。
（8）晶圓1之製造 藉由電漿CVD，於12英吋之矽晶圓上，依序成膜500 nm之SiO、50 nm之SiCN、250 nm之SiO。使用光罩，對表層之250 nm之SiO層進行蝕刻，之後，作為障壁金屬層，形成50 nm之Ta，進而於其上形成10 nm之TaN，然後進行鍍Cu，並藉由CMP進行平坦化，而製作電極圖案。藉由電漿CVD，於電極圖案上依序成膜SiCN層（50 nm）、SiO層（500 nm），而獲得具有電極之晶圓1。 （9）晶圓2之製造 以利用對向之接合電極及晶圓上形成之電極於貼合時形成菊鍊（daisy chain）之方式進行圖案加工，除此以外，藉由與晶圓1同樣之方式製作晶圓2。
（實施例1） 將所獲得之POSS-A 100重量份、作為觸媒之二月桂酸二丁基錫0.1重量份、作為交聯劑之矽酸酯MS51（Mitsubishi Chemical公司製造）1重量份溶解於丙二醇單乙基乙酸酯中，以樹脂固形物成分量成為50%之方式進行混合，藉此獲得硬化性樹脂組成物溶液。 繼而，利用旋轉塗佈機，將所獲得之硬化性樹脂組成物溶液塗佈於晶圓1之形成有電極之面，以70℃加熱30分鐘後，再以90℃加熱1小時，藉此進行溶劑乾燥，進而以200℃加熱1小時，藉此於晶圓1之電極面上形成厚度20 μm之有機膜。之後，藉由電漿CVD，成膜500 nm之SiN層。繼而，藉由使用光罩對SiN層及有機膜、以及晶圓1之電極面上存在之500 nm之SiO及50 nm之SiCN進行蝕刻，而於晶圓1之電極上形成貫通孔。此時，將蝕刻之通孔徑設為20 μm，將相鄰之通孔間的間距設為40 μm。之後，作為障壁金屬層，形成50 nm之Ta，進而於其上形成10 nm之TaN，繼而進行鍍Cu，藉此將導電性材料填充至貫通孔中。繼而，藉由對晶圓1之實施了鍍Cu之側之面（晶圓1之積層有機膜之側之面）進行研削，去除無用之障壁層及導電性材料，而形成接合電極。 另一方面，除以利用對向之電極形成菊鍊之方式進行圖案加工以外，與晶圓1同樣地，於晶圓2上亦形成有機膜及接合電極。 之後，對晶圓1及晶圓2進行H2 電漿清洗後，於真空中，以接合電極彼此重疊之方式將2片基板貼合，並進行400℃、4小時之加熱處理，藉此獲得積層體。
（實施例2～8） 除使硬化性樹脂之種類及觸媒之有無如表1所載以外，藉由與實施例1同樣之方式獲得積層體。 （實施例9） 將作為交聯劑之矽酸酯MS51（Mitsubishi Chemical公司製造）之含量設為3.2重量份，除此以外，藉由與實施例5同樣之方式獲得積層體。 （實施例10） 將作為交聯劑之矽酸酯MS51（Mitsubishi Chemical公司製造）之含量設為16重量份，除此以外，藉由與實施例5同樣之方式獲得積層體。 （實施例11） 將作為交聯劑之矽酸酯MS51（Mitsubishi Chemical公司製造）之含量設為32重量份，除此以外，藉由與實施例5同樣之方式獲得積層體。 （實施例12） 除於形成有機膜後不形成500 nm之SiN層以外，藉由與實施例1同樣之方式獲得積層體。
（比較例1） 藉由實施電漿CVD，於晶圓1之形成有電極之面，形成厚度20 μm之由Si3 N4 構成之無機層。以上述無機層代替有機膜，除此以外，藉由與實施例1同樣之方法獲得積層體。再者，電漿CVD之詳細條件如下。 原料氣體：SiH4 氣體及氮氣 流量：SiH4 氣體10 sccm、氮氣200 sccm RF功率：10 W（頻率2.45 GHz） 腔室內溫度：100℃ 腔室內壓力：0.9 Torr
（比較例2） 使用SiH4 氣體及氧氣作為原料氣體，將電漿CVD之靶變更為SiO2 ，形成厚度20 μm之由SiO2 構成之無機層，除此以外，藉由與比較例1同樣之方式獲得積層體。
（重量損失之測定） 藉由上述方法，分別製作有機膜及無機層之單層體。對於所獲得之單層體，使用示差熱-熱重量同步測定裝置（TG-DTA；STA7200，Hitachi High-Tech Science公司製造），於氮氣流（50 mL/min）下，以10℃/min之升溫速度自25℃加熱至400℃，並於400℃保持4小時，測定此時之重量損失率。將結果示於表1。
（表面硬度之測定） 將所獲得之積層體之側面包埋於冷樹脂中，並進行研削，於側面露出有機膜或無機層。繼而，使用奈米壓痕儀（TI 950 Tribo Indenter，Scienta Omicron公司製造），於以下條件下進行測定，藉此獲得有機膜或無機層之壓痕曲線：以測定位移200 nm/秒之速度將樣品壓入1000 nm，之後以200 nm/秒之速度拔出測定探針。再者，作為測定探針，使用Berkovich型金剛石壓頭。根據所獲得之壓痕曲線，基於ISO14577，算出表面之奈米壓痕硬度，藉此測得表面硬度。將與壓頭形狀有關之常數ε設為ε＝0.75。將結果示於表1。
（拉伸彈性模數之評價） 藉由上述方法，分別製作有機膜及無機層之單層體。藉由動態黏彈性測定裝置（IT計測控制公司（ITKDVA）製造，DVA-200），於定速升溫拉伸模式、升溫速度10℃/分鐘、頻率10 Hz之條件下測定所獲得之單層體之拉伸彈性模數。
＜評價＞ 對實施例及比較例中獲得之積層體進行以下評價。將結果示於表1。
（連接可靠性之評價） 確認實施例及比較例中獲得之積層體的晶圓中心部、距晶圓中心5 cm、10 cm之位置處之電極的電流導通情況，按照下述基準對初始連接可靠性進行評價。再者，各位置之電極係由10×10個電極構成之菊鍊。 ○：所有位置均於晶圓貼合後導通之情形 ×：晶圓貼合後存在導通不良部位之情形
繼而，以將積層體於－40℃放置30分鐘，然後升溫至125℃並放置30分鐘之操作為1組，實施100組或300組（可靠性試驗）後，進行與上述初始連接可靠性同樣之評價，以評價可靠性試驗後之連接可靠性。 ◎：300組後所有位置均導通之情形 ○： 100組後所有位置均導通但300組後存在導通不良部位之情形 ×：100組後存在導通不良部位之情形
（接著可靠性之評價） 利用超音波攝影裝置，測定配置於晶圓中心部、距晶圓中心5 cm、10 cm之位置的電極部之剝離面積。基於所獲得之剝離面積，按照以下基準對接著可靠性進行評價。再者，分別對上述可靠性試驗前（初始）及可靠性試驗（100組）後之積層體進行評價。 ◎：剝離面積未達5% ○：剝離面積為5%以上且未達30% ×：剝離面積為30%以上
[表1]
   實施例1 實施例2 實施例3 實施例4 實施例5 實施例6 實施例7 實施例8 實施例9 實施例10 實施例11 實施例12 比較例1 比較例2
硬化性樹脂 POSS-A POSS-A POSS-B POSS-C POSS-D POSS-E POSS-F PDMS樹脂 POSS-D POSS-D POSS-D POSS-A Si3 N4 SiO2
交聯劑 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 3.2 16.0 32.0 1.0 - -
觸媒 1.0 0.0 0.0 1.0 1.0 0.0 0.0 0.0 1.0 1.0 1.0 1.0 - -
重量損失(%) 3.0 5.0 ＞5.0 4.0 4.0 ＞5.0 ＞5.0 ＞10.0 4.0 6.0 8.0 3.0 0.0 0.0
表面硬度(GPa) 0.5 0.3 0.3 0.8 0.9 0.8 0.3 0.2 0.9 0.5 0.5 0.5 9.8 14.0
拉伸彈性模數(GPa) 0.4 0.3 0.2 0.5 0.7 0.5 0.4 0.2 0.9 0.6 0.6 0.4 70.0 290.0
無機層 有 有 有 有 有 有 有 有 有 有 有 無 有 有
連接可靠性 初始 ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○
可靠性試驗後 ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ◎ ○ × ×
接著可靠性 初始 ◎ ◎ ◎ ◎ ◎ ◎ ◎ ○ ◎ ◎ ◎ ◎ ◎ ◎
可靠性試驗後 ◎ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ ○ × ×
[產業上之可利用性]
根據本發明，可提供一種具有高電連接可靠性之積層體、用於該積層體之硬化性樹脂組成物、該積層體之製造方法、用於製造該積層體之具有接合電極之基板的製造方法、及具有該積層體之半導體裝置及攝影裝置。
1:第1基板 2:第2基板 3:電極 4:有機膜 5:貫通孔 6:無機層 7:障壁金屬層
[圖1]係示意性地表示本發明之積層體之一態樣的圖。 [圖2[係示意性地表示本發明之積層體之一態樣的圖。

Claims (22)

  1. 一種積層體，其依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，上述第1基板所具有之電極與上述第2基板所具有之電極經由貫通上述有機膜之貫通孔而電連接。
  2. 如請求項1之積層體，其中，上述有機膜於進行400℃、4小時之熱處理後，重量損失率為5%以下。
  3. 如請求項1或2之積層體，其中，上述有機膜之藉由奈米壓痕儀測得之表面硬度為5 GPa以下。
  4. 如請求項1至3中任一項之積層體，其中，上述有機膜為硬化性樹脂組成物之硬化物。
  5. 如請求項4之積層體，其中，上述有機膜含有有機矽化合物。
  6. 如請求項5之積層體，其中，上述有機矽化合物具有下述通式（1）所表示之結構：
    Figure 03_image001
    此處，R0 、R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫；上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基；m、n分別表示1以上之整數。
  7. 如請求項5或6之積層體，其中，上述有機矽化合物具有芳香環結構。
  8. 如請求項1至7中任一項之積層體，其中，上述有機膜含有促進硬化反應之觸媒。
  9. 如請求項1至8中任一項之積層體，其中，於上述第1基板與上述第2基板之間具有厚度1 nm以上1 μm以下之無機層。
  10. 如請求項1至9中任一項之積層體，其中，於上述貫通孔之表面具有障壁金屬層。
  11. 一種硬化性樹脂組成物，其用於形成如下積層體之有機膜，該積層體依序含有具有電極之第1基板、有機膜、及具有電極之第2基板，上述第1基板所具有之電極與第2基板所具有之電極經由貫通上述有機膜之貫通孔而電連接。
  12. 如請求項11之硬化性樹脂組成物，其中，上述硬化性樹脂組成物之硬化物於25℃之拉伸彈性模數為1 GPa以下。
  13. 如請求項11或12之硬化性樹脂組成物，其含有具有反應性部位之有機矽化合物。
  14. 如請求項13之硬化性樹脂組成物，其中，上述具有反應性部位之有機矽化合物具有下述通式（1）所表示之結構：
    Figure 03_image001
    此處，R0 、R1 及R2 分別獨立地表示直鏈狀、支鏈狀或環狀之脂肪族基、芳香族基或氫；上述脂肪族基及上述芳香族基可具有取代基，亦可不具有取代基；m、n分別表示1以上之整數。
  15. 如請求項13或14之硬化性樹脂組成物，其中，上述有機矽化合物具有芳香環結構。
  16. 如請求項13至15中任一項之硬化性樹脂組成物，其中，於硬化性樹脂組成物中之樹脂固形物成分量100重量份中，上述具有反應性部位之有機矽化合物之含量為90重量份以上98重量份以下。
  17. 如請求項11至16中任一項之硬化性樹脂組成物，其含有促進硬化反應之觸媒。
  18. 如請求項13至17中任一項之硬化性樹脂組成物，其含有多官能交聯劑，該多官能交聯劑可與上述具有反應性部位之有機矽化合物之反應性部位發生反應。
  19. 一種積層體之製造方法，其包括以下步驟： 於具有電極之第1基板的電極形成面上形成有機膜之步驟； 於上述有機膜形成貫通孔之步驟； 用導電性材料填充上述貫通孔之步驟； 對上述基板之填充有導電性材料之側之表面進行研磨而形成接合電極之步驟；以及 以上述接合電極彼此接合之方式，將形成有上述接合電極之上述第1基板與形成有上述接合電極之第2基板貼合之步驟。
  20. 一種具有接合電極之基板的製造方法，其包括以下步驟： 於具有電極之基板的電極形成面上形成有機膜之步驟； 於上述有機膜形成貫通孔之步驟； 用導電性材料填充上述貫通孔之步驟；以及 對上述基板之表面進行研磨而形成接合電極之步驟。
  21. 一種半導體裝置，其具有請求項1至10中任一項之積層體。
  22. 一種攝影裝置，其具有請求項1至10中任一項之積層體。
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