TWI608066B - 樹脂組成物、樹脂片及其製造方法、以及半導體裝置的製造方法 - Google Patents

樹脂組成物、樹脂片及其製造方法、以及半導體裝置的製造方法 Download PDF

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TWI608066B
TWI608066B TW103119969A TW103119969A TWI608066B TW I608066 B TWI608066 B TW I608066B TW 103119969 A TW103119969 A TW 103119969A TW 103119969 A TW103119969 A TW 103119969A TW I608066 B TWI608066 B TW I608066B
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resin sheet
resin composition
resin
weight
compound
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TW103119969A
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TW201500505A (zh
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榛葉陽一
松村和行
野中敏央
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東麗股份有限公司
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    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
    • B29C41/02—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor for making articles of definite length, i.e. discrete articles
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
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Description

樹脂組成物、樹脂片及其製造方法、以及半導體裝 置的製造方法
本發明是有關於一種樹脂組成物等，可用於個人電腦以及行動終端機等中使用的電子零件與印刷基板、可撓性基板等基板的黏接，以及電子零件彼此的黏接或基板彼此的黏接。更詳細而言，本發明是有關於當將積體電路(integrated circuit，IC)、大規模積體電路(large scale integration，LSI)等半導體晶片黏接於可撓性基板、玻璃環氧基板、玻璃基板、陶瓷基板、矽中介板(silicon interposer)等電路基板上時，或半導體晶片彼此的黏接或三維安裝等半導體晶片的積層時所使用的樹脂組成物等。另外，本發明還有關於用於製造增層多層基板等電路基板的絕緣層、抗蝕刻劑、阻焊劑等中可使用的樹脂組成物等。
近年來，隨著半導體裝置的小型化與高密度化，作為將半導體晶片安裝於電路基板上的方法，倒裝晶片安裝受到關注，並急速擴大。倒裝晶片安裝中，用以確保金屬電極的接合部分的 電性連接可靠性的方法通常採用使用樹脂組成物，將半導體晶片與電路基板黏接的方法。此處，使用樹脂組成物的黏接方法有以下方法：將包含溶劑的糊狀樹脂組成物塗佈於其中一個黏接對象物的表面，去除溶劑後，藉由加熱加壓來同時進行黏接對象物彼此的黏接與樹脂組成物的硬化的方法；或預先將糊狀的樹脂組成物塗佈於剝離性基材上後，去除溶劑來製作樹脂片，將其用於黏接對象物彼此的黏接的方法等。樹脂組成物的使用方法亦存在如下情況：於將導體層與絕緣層交替積層的增層多層基板的製造中，使用樹脂組成物的硬化物作為絕緣層。該些樹脂組成物正廣泛用於電氣．電子．建築．汽車．飛機等各種用途(例如參照專利文獻1~專利文獻2)。
考慮到室溫下的操作的容易度，所述樹脂片被設計成在室溫下不具有黏接性，但若加熱至100℃左右，則變得柔軟而具有黏接性。此處，藉由加熱而變得柔軟時的構成樹脂片的樹脂組成物的熔融黏度較佳為低。然而，樹脂片存在當保存時緩緩進行硬化而使熔融黏度提高的問題，期望保存穩定性的提高。對此，提出有如下技術，即，藉由使用微膠囊型硬化促進劑，來改良100℃以下的保存穩定性(例如，參照專利文獻3~專利文獻4)。
另外，因樹脂組成物的硬化物隨著溫度變化而大幅度伸縮，故於所得的半導體裝置內部產生應力，存在裝置的可靠性劣化的問題。對此，已知如下技術，即，為了使樹脂組成物的硬化物的線膨脹率接近於半導體晶片或電路基板的低的線膨脹率，而 於樹脂組成物中混合無機粒子(例如參照專利文獻1~專利文獻4)。
[現有技術文獻] [專利文獻]
[專利文獻1]日本專利特開平11-92549號公報
[專利文獻2]日本專利特開2011-95731號公報
[專利文獻3]日本專利特開2011-63678號公報
[專利文獻4]國際公開WO2012/043764號手冊
然而，關於經由現有的樹脂片而使半導體晶片彼此或者半導體晶片與基板黏接，進行金屬電極的接合來製作的半導體裝置，於熱循環試驗等中存在連接可靠性變得不良的情況。
本發明的目的在於提供一種樹脂片，其可提供於黏接及硬化後的樹脂片中抑制使連接可靠性惡化的氣泡或龜裂產生、且連接可靠性高的半導體裝置。
另外，混合有大量無機粒子的糊狀樹脂組成物存在於保存中緩緩產生凝聚物的問題。藉此，例如當將糊狀樹脂組成物成形為片狀的情況下，存在平坦性變差，電子零件或基板等的黏接無法良好地進行的情況。
本發明的另一目的為提供一種抑制凝聚物產生的樹脂組成物，且所述樹脂組成物可提供連接可靠性高的半導體裝置。
本發明為一種樹脂片，其在朝與面平行的方向施加動態剪切應變時的應力測定中，於溫度80℃、頻率0.5Hz下，應變的振幅為膜厚的10%時的損耗正切與該振幅為膜厚的0.1%時的損耗正切之差為1以上。
另外，本發明的另一態樣為一種樹脂組成物，其含有：(a)環氧化合物、(b)微膠囊型硬化促進劑、(c)無機粒子以及(d)通式(1)所表示的化合物。
所述通式(1)中，r、s及t分別表示0~2的整數。
另外，本發明的另一態樣為一種樹脂片的製造方法，其將所述樹脂組成物塗佈於剝離性基材上後，將揮發成分去除。
另外，本發明的另一態樣為一種半導體裝置的製造方法，其在第一電路構件與第二電路構件之間介隔所述樹脂片或者利用所述製造方法而獲得的樹脂片，藉由進行加熱加壓，使所述第一電路構件與所述第二電路構件電性連接。
藉由使用本發明的樹脂片，可提供於樹脂片中氣泡或龜 裂的產生少、連接可靠性優異的半導體裝置。另外，本發明的樹脂組成物於保存中凝聚物的產生少。另外，將該樹脂組成物成形為片狀而得的樹脂片的平坦性良好。另外，所述樹脂組成物的硬化物可提供連接可靠性高的電路基板或者半導體裝置。
本發明的樹脂片在朝與面平行的方向施加動態剪切應變時的應力測定(動態剪切應力測定)中的損耗正切的值滿足如下條件。即，於溫度80℃、頻率0.5Hz下，應變的振幅為膜厚的10%時的損耗正切、與該振幅為膜厚的0.1%時的損耗正切之差為1以上。以下，將該損耗正切之差稱為損耗正切差。
所謂動態剪切應力測定，是指以一定頻率對試樣賦予剪切應變，將其應力響應分解為對於應變的實部(彈性項)與虛部(黏性項)來進行評價。另外，所謂損耗正切，是指虛部相對於實部的比。評價裝置可列舉流變儀(rheometer)「AG-G2」(商品名，TA儀器(TA Instruments)公司製造)等。
通常，液狀物對於剪切應變而言，黏性佔支配地位。另一方面，硬化物對於剪切應變而言，彈性佔支配地位。如樹脂片之類的半固形物顯示黏性與彈性兩種性質。而且，將於剪切應變小的區域中為彈性、且於剪切應變大的區域中為黏性的性質稱為觸變性。本發明中，使用所述的損耗正切來定義樹脂片的觸變性， 並規定所需的範圍。損耗正切為黏性項相對於彈性項的比，因此隨著應變增加的損耗正切增加的程度顯示對象物的觸變性的程度。即，所述損耗正切差越大，樹脂片的觸變性越大。
發明者等人發現，於經由樹脂片而黏接半導體晶片或基板，並接合金屬電極的方法中，樹脂片的觸變性對連接可靠性的影響大。其原因並不明確，但認為：黏接時當金屬電極埋沒於樹脂片中時，於該金屬電極的附近區域，樹脂片的應變大，另一方面，於遠離金屬電極的區域，樹脂片的應變小；並且認為所述2個區域中的樹脂片的黏彈性的差異與連接的優劣有關。即認為，藉由樹脂片的觸變性，於應變大的金屬電極附近區域，樹脂片為黏性，因此金屬電極容易一邊推擠開樹脂片一邊埋沒於其中，相向的金屬電極彼此良好地抵接。另一方面認為，於遠離金屬電極的應變小的區域，樹脂片為彈性，因此藉由黏接時的壓力而容易將黏接時所捲入的氣泡擠出至外部或者使其消失。若於樹脂片中存在氣泡，則於對半導體裝置施加熱或衝擊的情況下，成為硬化後的樹脂片上產生龜裂的原因，由此，應力聚集於金屬電極的接合部，接合部斷裂，造成半導體裝置的連接可靠性的劣化。如此認為，藉由金屬電極的抵接以及氣泡的抑制兩種效果，半導體裝置的連接可靠性提高。
另外可知，觸變性高的樹脂片的平坦性高。其原因並不明確，但認為，若樹脂片或者樹脂組成物的觸變性高，則保存時材料中的黏度高，故而抑制凝聚物的產生，因此樹脂片的平坦性 提高。若樹脂片的平坦性良好，則半導體裝置的連接可靠性提高。
具體而言，於樹脂片的朝與面平行的方向的動態剪切應力測定中，於溫度80℃、頻率0.5Hz下，損耗正切差為1以上的情況下，使用該樹脂片來製作的半導體裝置的連接可靠性變得良好。損耗正切差更佳為1.5以上。另外，損耗正切差的上限並無特別限定，現實中多為5以下。
本發明的樹脂片於硬化後的朝與面平行的方向的動態黏彈性測定中(並非剪切應變，而是施加一維的動態應變的測定)，較佳為損耗正切顯示極大值時的溫度為160℃以上。其中，測定時的應變的振幅為膜厚的0.05%，頻率設為1Hz。評價裝置可列舉動態黏彈性測定裝置(動態力學分析(Dynamic Mechanical Analysis，DMA))「DVA-200」(商品名，IT計測控制(股)製造)等。
硬化後的樹脂片顯示彈性的行為，但若提高溫度，則於某溫度下，樹脂的主鏈開始振動，此時樹脂片的損耗正切顯示極大值。於該溫度以上，硬化後的樹脂片的黏性的性質提高。若損耗正切顯示極大值時的溫度為160℃以上，則使用樹脂片來製作的半導體裝置的連接可靠性提高。其原因並不明確，但認為，若損耗正切顯示極大值時的溫度低，則於熱循環試驗等伴隨加熱或冷卻的連接可靠性評價中，因在硬化後的樹脂片上產生黏性而於半導體裝置中產生應變，由此，應力聚集於硬化後的樹脂片或金屬接合部，產生龜裂或斷裂，半導體裝置的連接可靠性惡化。損耗 正切顯示極大值時的溫度尤佳為170℃以上。
本發明的樹脂片或者樹脂組成物是藉由加熱至100℃左右的溫度而產生流動性的半固形狀者。若將其進而加熱至100℃左右以上的溫度，則樹脂片或者樹脂組成物中的環氧化合物等樹脂成分進行交聯而形成網眼結構，藉此，流動性消失而成為固體狀。將該狀態變化稱為硬化，將所得者稱為樹脂片的硬化物或者樹脂組成物的硬化物。一旦硬化的硬化物恢復至室溫後，即便再次加熱，亦不會表現出流動性。硬化不僅藉由加熱來進行，而且亦有藉由紫外線等的照射來進行的情況。
本發明的樹脂片可藉由將含有溶劑的液體狀樹脂組成物塗佈於剝離性基材上，然後將溶劑等揮發成分去除來製作。
本發明的樹脂組成物含有(a)環氧化合物。(a)環氧化合物通常是藉由不伴隨收縮的開環而硬化，因此可減少樹脂組成物的硬化時的收縮。(a)環氧化合物較佳為具有2個以上環氧基的化合物、或環氧當量為100~500的化合物。若環氧當量為100以上，則樹脂組成物的硬化物的韌性變大。若環氧當量為500以下，則樹脂組成物的硬化物形成密度高的網眼結構，樹脂組成物的硬化物的絕緣性變得良好。
另外，(a)環氧化合物較佳為萘骨架環氧樹脂或者蒽骨架環氧樹脂。所謂萘骨架環氧樹脂或者蒽骨架環氧樹脂，是指具有萘骨架或者蒽骨架的環氧樹脂。藉由含有萘骨架環氧樹脂或者蒽骨架環氧樹脂，樹脂片以及樹脂組成物的觸變性提高，故而較 佳。另外，藉由含有萘骨架環氧樹脂或者蒽骨架環氧樹脂，樹脂片以及樹脂組成物的硬化物形成剛直的內部結構，故而顯示損耗正切的極大值時的溫度提高，因此使用其來製作的半導體裝置的連接可靠性提高，故而較佳。萘骨架環氧樹脂可列舉：愛匹克隆(Epiclon)(註冊商標)HP-4032、愛匹克隆(Epiclon)(註冊商標)HP-4700(以上為商品名，迪愛生(DIC)(股)製造)。另外，蒽骨架環氧樹脂可列舉jER(註冊商標)YX8800(商品名，三菱化學(股)製造)。
環氧化合物可列舉：jER(註冊商標)828、jER(註冊商標)152、jER(註冊商標)154、jER(註冊商標)630、jER(註冊商標)YL980、jER(註冊商標)1002、jER(註冊商標)1009、jER(註冊商標)5050、jER(註冊商標)YX4000、jER(註冊商標)YX4000UH、jER(註冊商標)YX8800(以上為商品名，三菱化學(股)製造)，EPPN(註冊商標)502H、NC-3000(以上為商品名，日本化藥(股)製造)，愛匹克隆(Epiclon)(註冊商標)N-695、愛匹克隆(Epiclon)(註冊商標)N-865、愛匹克隆(Epiclon)(註冊商標)HP-4032、愛匹克隆(Epiclon)(註冊商標)HP-4700、愛匹克隆(Epiclon)(註冊商標)HP-7200、愛匹克隆(Epiclon)(註冊商標)HP-7200H(以上為商品名，DIC(股)製造)，奧尼克斯(Aronix)(註冊商標)M-215、奧尼克斯(Aronix)(註冊商標)M315(以上為商品名，東亞合成(股)製造)，愛坡萊特(Epolite)1500 NP、愛坡萊特(Epolite)4000(以上為商品名，共榮社化學 (股)製造)等，但並不限定於該些化合物。亦可將該些組合2種以上。
當為了使本發明的樹脂片硬化而提高溫度時，(a)環氧化合物會對其黏彈性行為造成影響。若自室溫起不斷提高溫度，則樹脂片變得柔軟，黏度不斷下降，但黏度於100℃前後顯示最低點，且在此以上的溫度下不斷增加。其原因在於，樹脂片中的(a)環氧化合物開始硬化。將此時的黏度最低值稱為樹脂片的最低熔融黏度。例如，於經由樹脂片而使半導體晶片黏接於電路基板上的情況下，藉由形成於半導體晶片上的凸塊電極與電路基板的焊墊(pad)電極將樹脂片推擠開，凸塊電極與焊墊電極抵接而電性連接。若樹脂片的最低熔融黏度足夠低，則當經由樹脂片而將半導體晶片黏接於電路基板上時，半導體晶片或電路基板上的電極可容易地將樹脂片推擠開，對向的電極良好地抵接，因此在半導體晶片與電路基板的黏接的同時，確實地進行電極彼此的電性連接，電性連接可靠性提高，因此較佳。另外，若顯示最低熔融黏度時的溫度為100℃以上，則當將樹脂片在100℃以下的溫度下保存時，硬化難以進行，因此樹脂片的保存穩定性提高，故而較佳。
本發明的樹脂組成物含有(b)微膠囊型硬化促進劑。所謂微膠囊型硬化促進劑，是指以硬化促進劑作為芯成分，且將其周圍以微膠囊被覆而成者。(b)微膠囊型硬化促進劑由於藉由微膠囊來保護硬化促進劑，故而於100℃以下的溫度區域中抑制(a)環氧化合物的硬化，樹脂組成物的保存穩定性提高。
(b)微膠囊型硬化促進劑的芯成分可例示：二氰二胺(dicyandiamide)型硬化促進劑、胺加成物型硬化促進劑、有機酸醯肼型硬化促進劑、芳香族鋶鹽型硬化促進劑等。另外，被覆芯成分的微膠囊可例示：乙烯基系化合物、脲化合物、異氰酸酯化合物、熱塑性樹脂等。
相對於(a)環氧化合物100重量份，(b)微膠囊型硬化促進劑的含量較佳為0.1重量份~50重量份。若相對於(a)環氧化合物100重量份，(b)微膠囊型硬化促進劑的含量為0.1重量份以上，則使用樹脂組成物來製造的半導體裝置的連接可靠性提高。若相對於(a)環氧化合物100重量份，(b)微膠囊型硬化促進劑的含量為10重量份以上，則於低溫亦可以短時間來進行樹脂組成物的硬化，因此更佳。硬化溫度以及時間例如為160℃至200℃的溫度、且5秒至20分鐘，但並不限定於此。另外，若相對於(a)環氧化合物100重量份，(b)微膠囊型硬化促進劑的含量為50重量份以下，則樹脂組成物的100℃以下的保存穩定性提高。另外，樹脂組成物的硬化物的吸水性得以抑制，具有高強度以及高韌性，使用該樹脂組成物來製造的半導體裝置的連接可靠性提高。
(b)微膠囊型硬化促進劑較佳為使用對於樹脂組成物中所含的各成分並不溶解者。(b)微膠囊型硬化促進劑的具體例較佳為使用：將胺加成物型硬化促進劑以異氰酸酯化合物被覆而成的微膠囊型硬化促進劑，即諾巴固(Novacure)(註冊商標)HX-3941HP、諾巴固(Novacure)(註冊商標)HX-3922HP、諾巴 固(Novacure)(註冊商標)HX-3932HP、諾巴固(Novacure)(註冊商標)HX-3042HP(以上為商品名，旭化成電子材料(Asahi Kasei E-Materials)(股)製造)等。
此外，(b)微膠囊型硬化促進劑可使用以分散於液狀環氧化合物中的狀態而存在的硬化促進劑組成物。例如，作為市售的微膠囊型硬化促進劑的諾巴固(Novacure)(註冊商標)(商品名，旭化成電子材料(股)製造)系列是以相對於(b)微膠囊型硬化促進劑100重量份而包含環氧化合物200重量份的硬化促進劑組成物的形式來銷售。因此，於使用諾巴固(Novacure)(註冊商標)系列作為(b)微膠囊型硬化促進劑的情況下，在樹脂組成物中的各成分的含量的計算中，需要將硬化促進劑組成物中所含的環氧化合物合併作為(a)環氧化合物來計算。而且，自硬化促進劑組成物整體的重量中減去其中所含的環氧化合物的重量而得者為(b)微膠囊型硬化促進劑的重量。
(b)微膠囊型硬化促進劑的分散粒徑較佳為0.5μm~5μm。此處所謂分散粒徑，表示彼此在空間上分開存在的各(b)微膠囊型硬化促進劑的平均粒徑。於(b)微膠囊型硬化促進劑的形狀為球狀的情況下，將其直徑作為分散粒徑，於橢圓狀或者扁平狀的情況下，將粒子的最大長度作為分散粒徑。進而，於形狀為棒狀或者纖維狀的情況下，將長邊方向的最大長度作為分散粒徑。
另外，藉由減小包含(a)環氧化合物以及其他構成材料的媒質的折射率與(b)微膠囊型硬化促進劑的折射率之差，可提 高樹脂組成物或者樹脂片的光線透過率。
另外，除了(b)微膠囊型硬化促進劑以外，亦可使用其他的硬化促進劑。其他的硬化促進劑具體而言可列舉：胺系硬化促進劑、膦系硬化促進劑、鏻系硬化促進劑、鋶系硬化促進劑、錪系硬化促進劑等。
本發明的樹脂組成物含有(c)無機粒子。藉由含有無機粒子，則樹脂片的觸變性提高，故而使用樹脂片來製作的半導體裝置的連接可靠性提高。另外，樹脂組成物的硬化物的線膨脹率降低，接近於半導體晶片或電路基板的線膨脹率，因此使用樹脂組成物來製作的半導體裝置的連接可靠性提高。
(c)無機粒子的材質可將二氧化矽、氧化鋁、氧化鈦、氮化矽、氮化硼、氮化鋁、氧化鐵、玻璃或其他的金屬氧化物、金屬氮化物、金屬碳酸鹽、硫酸鋇等金屬硫酸鹽等單獨使用或者混合2種以上來使用。該些材質中，就低熱膨脹性、低吸水性以及高分散性的方面而言，特佳為可使用二氧化矽。
(c)無機粒子的表面若經矽烷偶合劑等化合物進行修飾，則(c)無機粒子於樹脂組成物或者樹脂片中的分散性提高，因此較佳。此處，所謂無機粒子的表面經特定的化合物進行修飾，表示於粒子表面的一部分或者全部中，該化合物藉由共價鍵或離子鍵等而與粒子表面的原子連接。例如，於使用下述所列舉的矽烷偶合劑作為進行表面修飾的化合物的情況下，粒子表面的羥基與矽烷偶合劑的矽烷醇基藉由脫水縮合而形成共價鍵。
矽烷偶合劑例如可列舉：乙烯基三甲氧基矽烷、乙烯基三乙氧基矽烷、3-縮水甘油氧基丙基三甲氧基矽烷、3-縮水甘油氧基丙基三乙氧基矽烷、3-丙烯醯氧基丙基三甲氧基矽烷、3-丙烯醯氧基丙基三乙氧基矽烷、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三乙氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三甲氧基矽烷、N-2-(胺基乙基)-3-胺基丙基三乙氧基矽烷、N-苯基-3-胺基丙基三甲氧基矽烷、3-異氰酸酯丙基三乙氧基矽烷、3-巰基丙基三甲氧基矽烷等。
尤其，若(c)無機粒子的表面經具有丙烯醯氧基或者甲基丙烯醯氧基的化合物進行修飾，則於環氧化合物的存在下的(c)無機粒子的分散性變得良好，樹脂片的最低熔融黏度降低，因此使用其來製作的半導體裝置的連接可靠性提高。所述矽烷偶合劑中較佳為使用3-丙烯醯氧基丙基三乙氧基矽烷、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三乙氧基矽烷。
(c)無機粒子的含量較佳為相對於樹脂組成物中的固體成分，即，自樹脂組成物中去除溶劑等揮發成分的全部成分的量而言的含量為40重量%~70重量%。若(c)無機粒子的該含量為40重量%以上，則使樹脂組成物加熱硬化時的發泡減少，且樹脂組成物的硬化物的線膨脹率降低，因此使用樹脂組成物來製造的半導體裝置的連接可靠性提高。尤其於對半導體裝置進行吸濕回流處理以及熱循環處理之類的需要更強的耐久性的處理的情況下，可保持良好的連接可靠性。
另外，於(c)無機粒子的該含量為70重量%以下的情況下，抑制樹脂組成物的最低熔融黏度增加，另外，由於(c)無機粒子均勻地分散於樹脂組成物中，故而於將樹脂組成物塗佈為片狀的情況下，獲得不存在膜厚不均或針孔、龜裂等的樹脂片。因此，使用所述樹脂片來製造的半導體裝置的連接可靠性提高。進而，藉由(c)無機粒子的均勻分散，樹脂片的光線透過性變得良好。
(c)無機粒子的形狀可為球狀、破碎狀、薄片狀等非球狀的任一種，球狀的(c)無機粒子由於容易在樹脂組成物中均勻分散，故而可較佳地使用。
另外，(c)無機粒子的分散粒徑較佳為300nm以下，更佳為1nm~300nm。若分散粒徑為1nm以上，則樹脂組成物的最低熔融黏度降低，藉此樹脂片成形時的表面平坦性提高，因此半導體晶片或電路基板的黏接變得良好。(c)無機粒子的分散粒徑尤佳為10nm以上。若分散粒徑為300nm以下，則樹脂片的觸變性提高，因此使用樹脂片來製作的半導體裝置的連接可靠性提高。另外，樹脂片的光線透過率提高，於黏接面形成有樹脂片的半導體晶片或電路基板上的對準標記(alignment mark)的視認性變得良好。(c)無機粒子的分散粒徑尤佳為200nm以下，最佳為100nm以下。
此外，所謂(c)無機粒子的分散粒徑，表示彼此在空間上分開存在的各(c)無機粒子的平均粒徑。於粒子的形狀為球狀 的情況下，將其直徑作為分散粒徑，於橢圓狀或者扁平狀的情況下，將粒子的最大長度作為分散粒徑。進而，於粒子的形狀為棒狀或者纖維狀的情況下，將長邊方向的最大長度作為分散粒徑。另外，多個粒子凝聚而形成1個粒子者中，將所述凝聚粒子的最大長度作為分散粒徑。
作為測定樹脂組成物或者樹脂片中的(c)無機粒子的分散粒徑的方法，可藉由如下方法來測定：利用掃描型電子顯微鏡(scanning electron microscope，SEM)來直接觀察粒子，計算100個粒子的粒徑的平均值。另外，分散液中的無機粒子的分散粒徑可使用作為動態光散射方式的粒徑測定裝置的希森美康(Sysmex)(股)製造的「Zetasizer Nano ZS」(商品名)等來測定。
本發明的樹脂組成物含有(d)通式(1)所表示的化合物。以下將該化合物(d)稱為二酮化合物A。
所述通式(1)中，r、s及t分別表示0~2的整數。
藉由含有(d)二酮化合物A，而於保存樹脂組成物時抑制凝聚物產生。凝聚物產生的原理並不確定，但可知，於進入至容器中的樹脂組成物的與空氣接觸的表面會產生凝聚物，另外，若對樹脂組成物進行加熱，則凝聚物產生變得顯著。根據該事實 來推定，於樹脂組成物的表面附近，溶劑向空氣中揮發而局部地出現溶劑不足的區域，於該區域，樹脂組成物中所含的組成物凝聚而作為固形物來析出。
相對於樹脂組成物的包含溶劑的總量，(d)二酮化合物A的含量較佳為0.1重量%~10重量%。若該含量為0.1重量%以上，則抑制樹脂組成物保存中的凝聚物產生。若該含量為10重量%以下，則可抑制樹脂組成物中的(a)環氧化合物的硬化，可提高樹脂組成物的保存穩定性。
(d)二酮化合物A的例子可列舉：雙乙醯(diacetyl)、乙醯丙酮、2,3-戊二酮、2,3-己二酮、3,4-己二酮、2,5-己二酮、2,6-庚二酮、3,5-庚二酮等，其中較佳為乙醯丙酮。
本發明的樹脂組成物若更含有(e)化合物，即，具有(e1)選自丙烯醯氧基及甲基丙烯醯氧基中的基團、以及(e2)選自羧基及羥基中的基團的化合物，則樹脂組成物的硬化物的斷裂伸長率變大，因此較佳。以下將該化合物(e)稱為酸性丙烯酸酯。
酸性丙烯酸酯的含量較佳為相對於樹脂組成物中的固體成分，即，自樹脂組成物中去除溶劑等揮發成分的全部成分的量的含量為0.1重量%~5重量%。若含量為0.1重量%以上，則樹脂組成物的硬化物的斷裂伸長率變大。另外，若含量為5重量%以下，則100℃以下的樹脂組成物的保存穩定性提高。
酸性丙烯酸酯的例子可列舉：丙烯酸2-羥基乙酯、甲基丙烯酸2-羥基乙酯、丙烯酸2-羥基丙酯、甲基丙烯酸2-羥基丙酯、 丙烯酸2-羥基丁酯、2-丙烯醯氧基乙基丁二酸、2-丙烯醯氧基乙基鄰苯二甲酸、2-丙烯醯氧基乙基六氫鄰苯二甲酸、2-丙烯醯氧基乙基-2-羥基乙基鄰苯二甲酸、丙烯酸2-羥基-3-苯氧基丙酯、甲基丙烯酸2-羥基-3-丙烯醯氧基丙酯等。另外，市售的酸性丙烯酸酯例如可列舉：HOA-MS、HOA-MPL、HOA-MPE、環氧酯(Epoxy Ester)3000A、環氧酯(Epoxy Ester)3002A、TATH05(下述式(2))(以上為商品名，共榮社化學(股)製造)、卡亞拉德(KAYARAD)(註冊商標)ZAR1395H、卡亞拉德(KAYARAD)(註冊商標)ZFR1401H(以上為商品名，日本化藥(股)製造)等。
本發明的樹脂組成物若更含有具有醯亞胺環的有機溶劑可溶性聚醯亞胺，則表現出良好的耐熱性以及耐化學品性，因此較佳。尤其藉由使用在有機溶劑可溶性聚醯亞胺的側鏈上具有至少一個可與環氧基進行反應的官能基的化合物，則於用以使樹脂組成物進行硬化的加熱時，促進環氧化合物的開環以及於聚醯亞胺中的加成反應，可獲得具有密度更高的網眼結構的樹脂組成物 的硬化物。可與環氧基進行反應的官能基可列舉酚性羥基、磺酸基以及硫醇基。此種聚醯亞胺的合成方法並不限定於以下的例子，例如可列舉如下方法：首先，使具有可與環氧基進行反應的基團的酸二酐與二胺進行反應而合成聚醯亞胺前驅物，繼而，使用一級單胺作為封端劑，進行該聚醯亞胺前驅物的末端修飾，然後進行150℃以上的加熱，來進行聚醯亞胺閉環。作為其他方法，可列舉如下方法：先使酸二酐與作為封端劑的一級單胺進行反應後，添加二胺而合成經末端修飾的聚醯亞胺前驅物，進而進行150℃以上的加熱，來進行聚醯亞胺閉環。
有機溶劑可溶性聚醯亞胺的較佳一例為具有下述通式(4)及通式(5)的任一者所表示的結構的聚合物。進而相對於聚合物總量，而具有5重量%~15重量%的通式(3)所表示的結構作為通式(4)及通式(5)中的R4。若通式(3)所表示的結構的該含量為5重量%以上，則聚醯亞胺可表現出適度的柔軟性，若該含量為15重量%以下，則確保聚醯亞胺的剛直性、耐熱性以及絕緣性。
式中，R1為2價烴基。R1較佳為碳數1~5的伸烷基、或者伸苯基。R2為1價烴基。R2較佳為碳數1~5的烷基、或者苯基。可於有機溶劑可溶性聚醯亞胺的1分子內包含不同結構的R1及R2。另外，亦可於有機溶劑可溶性聚醯亞胺的不同分子間包含不同結構的R1及R2。n表示1~10的整數，較佳為1~2。若n為1以上，則抑制硬化時的樹脂組成物的收縮，若為10以下，則聚醯亞胺骨架中的醯亞胺基含有率高，樹脂組成物的硬化物的絕緣性以及耐熱性變得良好。
式中，R3為4~14價有機基，R4為2~12價有機基。R3及R4的至少一個為含有至少一個選自由1,1,1,3,3,3-六氟丙基、異丙基、醚基、硫醚基以及SO2基所組成的組群中的基團(以下將其稱為「特定基」)的芳香族基。R5及R6表示選自由酚性羥基、 磺酸基以及硫醇基所組成的組群中的基團。可於有機溶劑可溶性聚醯亞胺的1分子內包含不同結構的R3~R6，亦可於有機溶劑可溶性聚醯亞胺的不同分子間包含不同的結構的R3~R6。X表示1價有機基。m為8~200，較佳為10~150。α及β分別表示0~10的整數，α+β為0~10的整數。其中，重複單元中，20%~90%為α+β=1~10。
此外，所謂有機溶劑可溶性聚醯亞胺的可溶性，是指在23℃下於選自以下的至少1種溶劑中溶解20重量%以上。酮系溶劑的丙酮、甲基乙基酮、甲基異丁基酮、環戊酮、環己酮；醚系溶劑的1,4-二噁烷、四氫呋喃、二甘二甲醚(diglyme)；二醇醚系溶劑的甲基溶纖劑、乙基溶纖劑、丙二醇單甲醚、丙二醇單乙醚、丙二醇單丁醚、二乙二醇甲基乙醚；此外，苄醇、N-甲基吡咯啶酮、γ-丁內酯、乙酸乙酯以及N,N-二甲基甲醯胺。
通式(4)及通式(5)中，R3表示酸二酐的殘基，較佳為碳數5~40的4~14價有機基。另外，R4表示二胺的殘基，較佳為碳數5~40的2~12價有機基。另外，較佳為R3及R4兩者含有至少一個所述特定基。
X為由作為封端劑的1級單胺而來的基團。X可為1種，亦可為2種以上的組合。具體而言，1級單胺可列舉：5-胺基喹啉、4-胺基喹啉、3-胺基萘、2-胺基萘、1-胺基萘、苯胺等。該些單胺中，特佳為使用苯胺。相對於全部二胺成分，聚合物中的X成分的含量較佳為0.1莫耳%~60莫耳%的範圍，特佳為5莫耳%~50 莫耳%。
另外，導入至聚合物中的通式(3)的結構以及封端劑可利用以下方法來容易地檢測、定量。例如，可藉由將導入有通式(3)的結構以及封端劑的聚合物溶解於酸性溶液或者鹼性溶液中，分解為作為聚合物的構成單元的二胺成分及酸酐成分，對其使用氣相層析法(gas chromatography，GC)、或核磁共振(nuclear magnetic resonance，NMR)進行測定，而容易地檢測、定量通式(3)的結構以及封端劑。除此以外，亦可藉由使用熱解氣相層析法(Pyrolysis-Gas Chromatography，PGC)或紅外光譜以及13C-NMR，對導入有封端劑的聚醯亞胺直接進行測定，而容易地檢測、定量通式(3)的結構以及封端劑。
有機溶劑可溶性聚醯亞胺可為僅包含通式(4)及通式(5)所表示的結構的化合物，亦可為含有其他結構的共聚物或者混合物。較佳為含有有機溶劑可溶性聚醯亞胺整體的50莫耳%以上的通式(4)及通式(5)所表示的結構。共聚物或者混合物中使用的其他結構的種類以及量較佳為於不會損及藉由加熱處理而獲得的樹脂組成物的硬化物的耐熱性的範圍內選擇。
有機溶劑可溶性聚醯亞胺是利用公知的方法來合成。例如可列舉利用以下方法獲得聚醯亞胺前驅物，繼而使所述聚醯亞胺前驅物進行公知的醯亞胺化反應的方法等，即：於低溫下使四羧酸二酐與二胺化合物進行反應的方法；藉由四羧酸二酐與醇的反應而獲得二酯，然後與二胺於縮合劑的存在下進行反應的方 法；藉由四羧酸二酐與醇的反應而獲得二酯，然後將殘留的二羧酸進行醯氯化，與二胺進行反應的方法等。
對所使用的酸二酐進行說明。具體而言，具有至少一個所述特定基的酸二酐可列舉：2,2-雙(3,4-二羧基苯基)丙烷二酐、2,2-雙(2,3-二羧基苯基)丙烷二酐、雙(3,4-二羧基苯基)碸二酐、雙(3,4-二羧基苯基)醚二酐、2,2-雙(3,4-二羧基苯基)六氟丙烷二酐、或者於該些化合物的芳香族環上具有烷基或鹵素原子的取代基的化合物等。
另外，亦可使用所述以外的酸二酐，具體而言為：均苯四甲酸二酐、3,3',4,4'-聯苯四羧酸二酐、2,3,3',4'-聯苯四羧酸二酐、2,2',3,3'-聯苯四羧酸二酐、3,3',4,4'-二苯甲酮四羧酸二酐、2,2',3,3'-二苯甲酮四羧酸二酐、1,1-雙(3,4-二羧基苯基)乙烷二酐、1,1-雙(2,3-二羧基苯基)乙烷二酐、雙(3,4-二羧基苯基)甲烷二酐、雙(2,3-二羧基苯基)甲烷二酐、1,2,5,6-萘四羧酸二酐、2,3,6,7-萘四羧酸二酐、2,3,5,6-吡啶四羧酸二酐、3,4,9,10-苝四羧酸二酐等芳香族四羧酸二酐、或者於該些化合物的芳香族環上具有烷基或鹵素原子的取代基的化合物等。該些酸二酐可單獨使用或者將2種以上組合使用。
對所使用的二胺進行說明。具體而言，具有至少一個所述特定基的二胺可列舉：3,4'-二胺基二苯基硫醚、4,4'-二胺基二苯基硫醚、3,4'-二胺基二苯基醚、4,4'-二胺基二苯基醚、3,4'-二胺基二苯基碸、4,4'-二胺基二苯基碸、雙[4-(4-胺基苯氧基)苯基]碸、 雙[4-(3-胺基苯氧基)苯基]碸、雙(4-胺基苯氧基)聯苯、雙[4-(4-胺基苯氧基)苯基]醚、1,4-雙(4-胺基苯氧基)苯、1,3-雙(4-胺基苯氧基)苯、2,2-雙[4-(4-胺基苯氧基)苯基]六氟丙烷、2,2-雙[4-(4-胺基苯氧基)苯基]丙烷、或者於該些化合物的芳香族環上具有烷基或鹵素原子的取代基的化合物等。
具體而言，具有至少一個所述特定基且具有至少一個選自由酚性羥基、磺酸基以及硫醇基所組成的組群中的基團的二胺可列舉：2,2-雙(3-胺基-4-羥基苯基)六氟丙烷、2,2-雙(3-羥基-4-胺基苯基)六氟丙烷、2,2-雙(3-胺基-4-羥基苯基)丙烷、2,2-雙(3-羥基-4-胺基苯基)丙烷、3,3'-二胺基-4,4'-二羥基二苯基醚、3,3'-二胺基-4,4'-二羥基二苯基碸、3,3'-二胺基-4,4'-二羥基二苯基硫醚、或者於該些化合物的芳香族環上具有烷基或鹵素原子的取代基的化合物等。
另外，亦可使用所述以外的二胺，具體而言為：3,3'-二胺基-4,4'-二羥基聯苯、2,4-二胺基-苯酚、2,5-二胺基苯酚、1,4-二胺基-2,5-二羥基苯、二胺基二羥基嘧啶、二胺基二羥基吡啶、羥基二胺基嘧啶、9,9-雙(3-胺基-4-羥基苯基)茀、3,4'-二胺基二苯基甲烷、4,4'-二胺基二苯基甲烷、聯苯胺、間苯二胺、對苯二胺、1,5-萘二胺、2,6-萘二胺、2,2'-二甲基-4,4'-二胺基聯苯、2,2'-二乙基-4,4'-二胺基聯苯、3,3'-二甲基-4,4'-二胺基聯苯、3,3'-二乙基-4,4'-二胺基聯苯、2,2',3,3'-四甲基-4,4'-二胺基聯苯、3,3',5,5'-四甲基-4,4'-二胺基聯苯、2,2'-二(三氟甲基)-4,4'-二胺基聯苯、或者於該 些化合物的芳香族環上具有烷基或鹵素原子的取代基的化合物，或對苯二甲酸醯肼、間苯二甲酸醯肼、鄰苯二甲酸醯肼、2,6-萘二羧酸二醯肼、4,4'-雙苯基二羰肼(4,4'-bisphenyl dicarbonohydrazine)、4,4'-環己烷二羰肼、或者於該些化合物的芳香族環上具有烷基或鹵素原子的取代基的醯肼化合物等。該些二胺可單獨使用或者將2種以上組合使用。
另外，包含通式(3)所表示的結構的二胺可列舉：雙(3-胺基丙基)四甲基二矽氧烷、雙(對胺基-苯基)八甲基五矽氧烷等。
於將自樹脂組成物中去除溶劑及無機粒子而得的成分的量設為100重量份的情況下，有機溶劑可溶性聚醯亞胺的含量較佳為10重量份~20重量份。若有機溶劑可溶性聚醯亞胺的該含量為10重量份以上，則樹脂組成物的硬化物的耐熱性變得良好。另一方面，若有機溶劑可溶性聚醯亞胺的該含量為20重量份以下，則樹脂組成物的硬化物的吸水性降低，因此電路基板與半導體晶片間的黏接力增加，連接可靠性提高。另外，樹脂組成物的硬化物的絕緣性提高。另外，若有機溶劑可溶性聚醯亞胺的該含量為10重量份~20重量份，則樹脂片的最低熔融黏度低，此時的溫度提高，故而較佳。
本發明的樹脂組成物可出於硬化後的狀態下的低應力化的目的而更含有熱塑性樹脂。熱塑性樹脂例如可列舉：苯氧基樹脂、聚酯、聚胺基甲酸酯、聚醯胺、聚丙烯、丙烯腈-丁二烯共聚物(NBR)、苯乙烯-丁二烯共聚物(SBR)、丙烯腈-丁二烯-甲基 丙烯酸共聚物、丙烯腈-丁二烯-丙烯酸共聚物等，但並不限定於該些樹脂。
本發明的樹脂組成物亦可含有提高觸變性的化合物。提高觸變性的化合物可列舉：聚醚系、聚酯系等界面活性劑，或醯胺系、脂肪酸醯胺系、脲系等觸變性促進劑等。具體而言，可列舉：BYK(註冊商標)-405、BYK(註冊商標)-410、BYK(註冊商標)-411(以上為商品名，日本畢克化學(BYK-Chemie Japan)(股)製造)，帝司巴隆(Disparlon)(註冊商標)3600N、帝司巴隆(Disparlon)(註冊商標)3900EF、帝司巴隆(Disparlon)(註冊商標)6900-10X(以上為商品名，楠本化成(股)製造)等。
本發明的樹脂組成物可含有溶劑。溶劑可將以下化合物單獨使用或者混合使用2種以上：酮系溶劑的丙酮、甲基乙基酮、甲基異丁基酮、環戊酮、環己酮；醚系溶劑的1,4-二噁烷、四氫呋喃、二甘二甲醚；二醇醚系溶劑的甲基溶纖劑、乙基溶纖劑、丙二醇單甲醚、丙二醇單乙醚、丙二醇單丁醚、丙二醇單甲醚乙酸酯、丙二醇單乙醚乙酸酯、二乙二醇甲基乙醚；除此以外的苄基醇、N-甲基吡咯啶酮、γ-丁內酯、乙酸乙酯、N,N-二甲基甲醯胺等；但並不限定於該些溶劑。
以下，對本發明的樹脂組成物以及樹脂片的製造方法的例子進行詳細說明。
首先，將(a)環氧化合物、(b)微膠囊型硬化促進劑、(c)無機粒子、(d)二酮化合物A、(e)酸性丙烯酸酯、有機溶 劑可溶性聚醯亞胺、溶劑、聚合抑制劑、塑化劑、界面活性劑、調平劑、離子捕捉劑、矽烷偶合劑等進行混合而獲得樹脂組成物。
(c)無機粒子可使用1次粒子凝聚而成的粉體狀粒子，亦可使用(c)無機粒子的分散液。
於利用矽烷偶合劑等化合物對(c)無機粒子的表面進行修飾的情況下，例如以如下方式進行。將1次粒子凝聚而成的粉體狀的(c)無機粒子與溶劑混合，利用均質機、球磨機、珠磨機等分散裝置，將凝聚的(c)無機粒子拆解或粉碎而溶解於溶劑中。接著，於所得的(c)無機粒子的分散液中混合用以進行表面修飾的矽烷偶合劑等化合物，於室溫或者100℃以下的溫度下攪拌數小時，藉此獲得經表面修飾的(c)無機粒子的分散液。亦可於(c)無機粒子的分散前，預先將表面修飾用的化合物混合於溶劑中，而使(c)無機粒子的分散處理與表面處理同時進行。另外，亦可混合分散劑或消泡劑等其他化合物。可將經表面修飾的(c)無機粒子的分散液直接使用來製作樹脂組成物，亦可使用旋轉蒸發器等，自分散液中去除溶劑，使用所得的無機粒子的粉體來製作樹脂組成物。
進行所述材料的混合時，可使用均質機、球磨機、珠磨機等。由於在混合處理中存在因(b)微膠囊型硬化促進劑被破壞等，而(a)環氧化合物硬化的情況，因此(b)微膠囊型硬化促進劑較佳為於混合其他材料後添加，以比較弱的力來混合。
繼而，可藉由將以所述方式獲得的樹脂組成物塗佈於剝 離性基材上後，去除揮發成分而獲得樹脂片。具體而言，首先，使用棒式塗佈機、網版印刷、刀片塗佈機、模式塗佈機、缺角輪塗佈機等裝置，將樹脂組成物塗佈於剝離性基材上後，去除溶劑而獲得樹脂片。剝離性基材可列舉：聚對苯二甲酸乙二酯膜、聚萘二甲酸乙二酯膜、聚酯膜、聚氯乙烯膜、聚碳酸酯膜、聚醯亞胺膜、聚四氟乙烯膜等氟樹脂膜、聚苯硫醚膜、聚丙烯膜、聚乙烯膜等，但並不限定於該些膜。另外，剝離性基材亦可利用矽酮系、長鏈烷基系、氟系、脂肪族醯胺系等脫模劑來實施表面處理。剝離性基材的厚度並無特別限定，通常較佳為5μm~75μm。
將溶劑等揮發成分去除的方法較佳為藉由加熱處理來進行。作為加熱處理，除了利用烘箱或加熱板的加熱以外，可列舉利用真空乾燥、紅外線或微波等電磁波的加熱等。此處，於溶劑的去除不充分的情況下，經由樹脂片而黏接半導體晶片或電路基板後，藉由進一步的高溫加熱而使樹脂片硬化時，存在產生氣泡，黏接力下降的情況。另一方面，若過度進行用以去除溶劑的加熱，則存在樹脂片進行硬化，黏接力下降的情況。
較佳為於所得樹脂片的與具有剝離性基材的面為相反側的面上進而貼合另一剝離性基材，將樹脂片的兩面以剝離性基材夾持。另一剝離性基材的材質以及厚度可使用與先前所說明的剝離性基材相同的材質及厚度。兩剝離性基材可相同。但，各個剝離性基材與樹脂片間的黏接力較佳為存在差。黏接力之差特佳為5N/m~47N/m。藉由將黏接力之差設為5N/m以上，則當將黏接力 小的剝離性基材剝離時，可使樹脂片不會自另一剝離性基材上剝離或浮起。另外，藉由將黏接力之差設為47N/m以下，則於剝離後的各剝離性基材的表面難以殘存樹脂片。先塗佈樹脂組成物的剝離性基材的黏接力可大於、亦可小於之後貼合的剝離性基材的黏接力。
樹脂片的最低熔融黏度較佳為在10Pa．s~10000Pa．s的範圍內。更佳的最低熔融黏度的範圍為100Pa．s~5000Pa．s。若最低熔融黏度為該範圍，則除了所述電極的連接變得良好以外，可於無皺褶或氣泡捲入的情況下將樹脂片貼合於半導體晶圓或電路基板上，進而可減少半導體晶片安裝時的樹脂片的露出。此外，樹脂片的最低熔融黏度可使用例如流變儀「AG-G2」(商品名，TA儀器公司製造)，對尺寸為直徑15mm、厚度0.8mm的試樣，以測定頻率0.5Hz、升溫速度2℃/分鐘、測定溫度範圍40℃至150℃來測定。
對使用本發明的樹脂組成物的半導體裝置的製造方法進行說明。本發明的半導體裝置的製造方法是於第一電路構件與第二電路構件之間介隔本發明的樹脂組成物，藉由加熱加壓而使所述第一電路構件與所述第二電路構件電性連接的半導體裝置的製造方法。另外，較佳為使用藉由本發明的製造方法而獲得的樹脂片作為本發明的樹脂組成物。
具體而言，首先將具有第一電極的第一電路構件、與具有第二電極的第二電路構件，以第一電極與第二電極對向的方式 進行配置。繼而，於所述對向配置的第一電路構件與第二電路構件之間介隔本發明的樹脂組成物。此處，作為介隔樹脂組成物的方法，可於電路構件的表面直接塗佈樹脂組成物後將揮發成分去除，亦可於電路構件的表面貼合本發明的樹脂片。樹脂組成物可僅形成於任一電路構件的電極側的面上，亦可形成於第一電路構件以及第二電路構件兩者的電極側的面上。接著，對所述構件進行加熱加壓，而使第一電路構件與第二電路構件黏接，同時使所述對向配置的第一電極與第二電極電性連接。電極彼此的電性連接可藉由力學性按壓來進行，亦可藉由使用焊料等的金屬接合來進行。另外，亦可於第一電路構件及/或第二電路構件中形成貫通電極，於電路構件的單面及/或兩面形成電極。
以下，對使用樹脂片的情況的例子進行說明。藉由使用該方法，可利用樹脂組成物的硬化物，將半導體晶片與形成有配線圖案的電路基板之間的空隙密封。
首先，將樹脂片切出為既定的大小，貼合於形成有配線圖案的電路基板的配線圖案面上。或者，亦可藉由在切出半導體晶片之前的半導體晶圓的凸塊形成面上貼合樹脂片後，對半導體晶圓進行切割而單片化，來製作貼附有樹脂片的半導體晶片。樹脂片的貼合可使用輥式貼合機或真空貼合機等貼合裝置來進行。
將樹脂片貼合於電路基板或者半導體晶片上後，使用黏合裝置來安裝於半導體晶片的電路基板上。黏合條件只要是獲得良好的電性連接的範圍，則並無特別限定，但為了進行樹脂片的 硬化，較佳為以溫度為100℃以上、壓力為1mN/凸塊以上、時間為0.1秒以上的加熱加壓條件來黏合。以更佳為120℃以上、300℃以下，尤佳為150℃以上、250℃以下的溫度，且更佳為5mN/凸塊以上、50000mN/凸塊以下，尤佳為10mN/凸塊以上、10000mN/凸塊以下的壓力，以及更佳為1秒以上、60秒以下，尤佳為2秒以上、30秒以下的時間下的黏合條件來進行。另外，黏合時，作為暫時壓接，亦較佳為藉由溫度為50℃以上、壓力為1mN/凸塊以上、時間為0.1秒以上的加熱加壓，使半導體晶片上的凸塊與電路基板上的焊墊電極接觸後，以所述條件進行黏合。視需要，亦可於進行黏合後，將帶有半導體晶片的電路基板於50℃以上、200℃以下的溫度下加熱10秒以上、24小時以下。
為了獲得連接可靠性高的半導體裝置，較佳為於黏合後的樹脂組成物中無氣泡。為了獲得此種半導體裝置，有效的是於黏合時對半導體晶片施加高壓力。然而，於對半導體晶片施加高壓力的情況下，會導致半導體晶片的破損，因此先前不實施高壓力下的黏合。於使用本發明的樹脂片或者樹脂組成物的情況下可確認，即便以200N以上的高壓力來實施黏合，亦無半導體晶片的破損且將樹脂組成物中的氣泡去除。其原因並未確定，但推測為：於使用本發明的樹脂片或者樹脂組成物的情況下，對半導體晶片施加的壓力並非局部地施加於半導體晶片的一部分，而是均勻地按壓，藉此不會產生半導體晶片的破損。其中，就不會出現半導體晶片的破損，而且抑制半導體裝置的內部結構的不良的方 面而言，黏合時的壓力較佳為500N以下。
本發明的樹脂片以及樹脂組成物可適宜用於構成半導體裝置的電路構件彼此的黏接、固定或者密封。另外，可用於構成增層多層基板等電路基板的絕緣層、永久抗蝕劑、阻焊劑、密封劑等，或用於製造半導體裝置的抗蝕刻劑等。此處，所謂電路構件，是指構成半導體裝置的半導體晶片、晶片零件、電路基板、金屬配線材料等構件。電路構件的具體例可列舉：形成有鍍敷凸塊或柱形凸塊(stud bump)等凸塊的半導體晶片、電阻晶片或電容器晶片等晶片零件、具有矽穿孔(Through Silicon Via，TSV)電極的半導體晶片以及矽中介板等。此外，本發明中所謂的半導體裝置，是指可藉由利用半導體元件的特性來發揮功能的裝置整體，半導體電路以及電子設備全部包含於半導體裝置中。
另外，除了所述以外，本發明的樹脂片以及樹脂組成物亦可用作用以製作黏晶膜(die attach film)、切晶黏晶膜(dicing die attach film)、引線框架固定帶、散熱板、增強板、屏蔽材料的黏接劑、阻焊劑等的樹脂組成物。
[實施例]
以下列舉實施例等來對本發明進行說明，但本發明並不限定於該些例子。
<樹脂片的最低熔融黏度的測定方法>
使用流變儀「AG-G2」(商品名，TA儀器公司製造)來測定樹脂片的黏彈性特性。首先，藉由在80℃的加熱板上重疊貼合多 片樹脂片而製作厚度為0.8mm的樹脂片，切出為直徑為15mm的圓形而作為試驗片。測定條件為：以升溫速度2℃/分鐘、剪切應變的振幅相對於膜厚而為10%、測定頻率0.5Hz的條件，一邊自40℃升溫至150℃一邊進行測定。測定複數黏度(complex viscosity)，讀取在測定範圍內最低的複數黏度的值作為最低熔融黏度。
<樹脂片的損耗正切差的測定方法>
使用流變儀「AG-G2」(商品名，TA儀器公司製造)來測定樹脂片的損耗正切差。首先，藉由在80℃的加熱板上重疊貼合多片樹脂片而製作厚度為0.8mm的樹脂片，將其切出為直徑為15mm的圓形而作為試驗片。測定條件為：以溫度80℃、測定頻率0.5Hz，一邊使剪切應變的振幅相對於膜厚而自0.01%變化至100%一邊進行測定。算出應變振幅為10%時的損耗正切、與應變振幅為0.1%時的損耗正切之差。
<樹脂片的硬化物的損耗正切極大時溫度的測定方法>
使用動態黏彈性測定裝置(DMA)「DVA-200」(商品名，IT計測控制(股)製造)來測定樹脂片的硬化物的損耗正切的極大值下的溫度。首先，藉由在80℃的加熱板上重疊貼合多片硬化前的樹脂片而製作厚度為0.5mm的樹脂片。於180℃下進行2小時加熱處理，使樹脂片硬化。繼而，以形狀成為5mm×40mm的長條狀的方式將硬化後的樹脂片切斷而作為試驗片。測定條件為：以測定頻率1Hz、應變振幅0.05%、升溫速度5℃/分鐘， 一邊使溫度自40℃變化至300℃一邊進行測定。測定後，讀取損耗正切顯示極大值時的溫度。
<樹脂片的硬化物中的無機粒子的分散粒徑的測定方法>
利用超薄切片法，將樹脂片的硬化物切出為厚度100nm的薄膜，使用穿透型電子顯微鏡H-7100FA(日立製作所(股)製造)來觀察樹脂片的硬化物中的無機粒子。倍率設為5萬倍。其中，對於實施例41~實施例42、比較例2，倍率設為5000倍。加速電壓設為100kV。將所得的觀察像作為數位影像而輸入電腦中，使用影像處理軟體FlvFs(弗羅貝爾(Flovel)(股)製造)，對所觀察到的任意100個粒子求出球形近似時的粒徑。將以所述方式求出的100個粒子的粒徑加以平均而得的平均粒徑作為分散粒徑。此外，於1次粒子凝聚而存在的情況下，測定凝聚體的粒徑。
除此以外，實施例、比較例中使用的各材料為如以下所述。
(a)環氧化合物
愛匹克隆(Epiclon)(註冊商標)HP-4700(商品名，基本骨架：萘，DIC(股)製造)
愛匹克隆(Epiclon)(註冊商標)HP-7200H(商品名，基本骨架：二環戊二烯，DIC(股)製造)
愛匹克隆(Epiclon)(註冊商標)HP-4032(商品名，基本骨架：萘，DIC(股)製造)
jER(註冊商標)YL980(商品名，185g/eq、基本骨架：雙酚A，三菱化學(股)製造)
jER(註冊商標)152(商品名，基本骨架：苯酚酚醛清漆，三菱化學(股)製造)
jER(註冊商標)8800(商品名，基本骨架：蒽，三菱化學(股)製造)
愛坡萊特(Epolite)4000(商品名，基本骨架：氫化雙酚A，共榮社化學(股)製造)。
(b)微膠囊型硬化促進劑
諾巴固(Novacure)(註冊商標)HX-3941HP(商品名，旭化成電子材料(股)製造)：諾巴固(Novacure)(註冊商標)HX-3941HP是微膠囊型硬化促進劑/環氧化合物為1/2，所含的環氧化合物為雙酚A型環氧化合物/雙酚F型環氧化合物=1/4。
(c)無機粒子
YA050C-SM1(商品名，亞都瑪科技(Admatechs)(股)製造，球形二氧化矽粒子，利用3-甲基丙烯醯氧基丙基三甲氧基矽烷進行表面處理，平均一次粒徑為50nm)
YA050C-SV2(商品名，亞都瑪科技(Admatechs)(股)製造，球形二氧化矽粒子，利用乙烯基三甲氧基矽烷進行表面處理，平均一次粒徑為50nm)
YA050C-SP3(商品名，亞都瑪科技(Admatechs)(股)製造，球形二氧化矽粒子，利用苯基三甲氧基矽烷進行表面處理，平均 一次粒徑為50nm)。
無機粒子A
將二氧化矽粒子的分散液「MEK-AC-5140Z」(商品名，日產化學工業(股)製造，球形二氧化矽粒子，平均一次粒徑為80nm，利用3-甲基丙烯醯氧基丙基三甲氧基矽烷進行表面處理，二氧化矽濃度為40重量%的甲基乙基酮分散液)300mL投入至500mL的茄型燒瓶中，使用旋轉蒸發器來去除溶劑，於80℃下乾燥3小時，獲得粉體的無機粒子A。
無機粒子B
將二氧化矽粒子的分散液「SE2050-KNK」(商品名，亞都瑪科技(Admatechs)(股)製造，球形二氧化矽粒子，平均一次粒徑為500nm，利用N-苯基-3-胺基丙基三甲氧基矽烷進行表面處理，二氧化矽濃度為70重量%的甲基異丁基酮分散液)300mL投入至500mL的茄型燒瓶中，使用旋轉蒸發器來去除溶劑，於80℃下乾燥3小時，獲得粉體的無機粒子B。
關於以上的無機粒子的表面處理，雖已示於製品規格中，但重新使用傅立葉變換紅外分光裝置「IR Prestige-21」(商品名，島津製作所(股)製造)來進行組成分析，確認到規格正確。
(d)通式(1)所表示的二酮化合物
雙乙醯(通式(1)中，r=0，s=0，t=0)
乙醯丙酮(通式(1)中，r=0，s=1，t=0)
2,5-己二酮(通式(1)中，r=0，s=2，t=0)
3,4-己二酮(通式(1)中，r=1、s=0，t=1)
(d')其他的二酮化合物
1,3-環己二酮
(e)酸性丙烯酸酯
HOA-MPL(商品名，共榮社化學(股)製造)
TATH05(下述式(2))(商品名，共榮社化學(股)製造)
(f)有機溶劑可溶性聚醯亞胺
有機溶劑可溶性聚醯亞胺A
於乾燥氮氣流下，使1,3-雙(3-胺基苯氧基)苯(以下稱為APB-N)4.82g(0.0165莫耳)、3,3'-二胺基-4,4'-二羥基二苯基碸(以下稱為ABPS)3.08g(0.011莫耳)、1,3-雙(3-胺基丙基)四甲 基二矽氧烷(以下稱為SiDA)4.97g(0.02莫耳)、以及作為封端劑的苯胺0.47g(0.005莫耳)，溶解於N-甲基-2-吡咯啶酮(以下稱為NMP)130g中。向其中添加20g的NMP，並且添加2,2-雙{4-(3,4-二羧基苯氧基)苯基}丙烷二酐(以下稱為BSAA)26.02g(0.05莫耳)，於25℃下進行1小時反應，繼而於50℃下攪拌4小時。然後，於180℃下進而攪拌5小時。攪拌結束後，將溶液投入至水3L中，進行過濾並回收沈澱物。將所得的沈澱物以水清洗3次後，使用真空乾燥機，於80℃下乾燥20小時。對所得的聚合物固體進行紅外分光測定，結果於1780cm-1附近、1377cm-1附近檢測出由聚醯亞胺引起的醯亞胺結構的吸收峰值。以所述方式獲得具有可與環氧基進行反應的官能基、且包含11.6重量%的通式(3)所表示的結構的有機溶劑可溶性聚醯亞胺A。於4g的有機溶劑可溶性聚醯亞胺A中添加四氫呋喃6g，於23℃下進行攪拌而溶解。
(g)觸變性促進劑
BYK(註冊商標)-410(商品名，日本畢克化學(股)製造)
帝司巴隆(Disparlon)(註冊商標)6900-10X(商品名，楠本化成(股)製造)
(h)溶劑
丙二醇單甲醚乙酸酯(簡稱為PGMEA)
環己酮
甲基異丁基酮(簡稱為MIBK)
丙二醇單甲醚(簡稱為PGME)。
實施例1
(1)樹脂組成物的製作
以成為表1所示的組成比的方式將(a)成分~(h)成分調合，使用球磨機，為了使材料均勻混合而進行10小時的處理，製作樹脂組成物。球磨機中使用直徑為5mm的氧化鋯球「YTZ(註冊商標)球」(商品名，尼卡特(Nikkato)(股)製造)。球磨機處理後，利用篩來去除氧化鋯球，獲得樹脂組成物。
(2)樹脂片的製作與評價
以所述方式製作樹脂組成物，於室溫下靜置30分鐘來保存後，使用棒式塗佈機，塗佈於作為剝離性基材的厚度為75μm的脫模膜「SR-1」(商品名，大槻工業(股)製造)上，於80℃下進行10分鐘乾燥而製作樹脂片。此處，以乾燥後的樹脂片的厚度成為50μm的方式調節塗佈厚度。利用光學顯微鏡來觀察樹脂片的表面的狀態，於10cm×10cm的正方形區域中數出50μm以上大小的凝聚物的數量，作為樹脂片的平坦性的指標。評價基準如以下所述，將其結果示於表1中。
A：未觀察到50μm以上大小的凝聚物。
B：觀察到1個~9個的50μm以上大小的凝聚物。
C：觀察到10個以上的50μm以上大小的凝聚物。
另外，製作所述樹脂組成物後，於室溫下靜置10小時來保存後，以與所述同樣的方法製作樹脂片，評價平坦性。將結果 示於表1中。
繼而，對於由在室溫下靜置10小時的樹脂組成物來製作的樹脂片，於樹脂片的與所述脫模膜「SR-1」為相反側的面上，貼合厚度為38μm的脫模膜「SR-3」(商品名，大槻工業(股)製造)作為另一剝離性基材，獲得於兩面具有剝離性基材的樹脂片。
測定所得樹脂片的最低熔融黏度與損耗正切差、以及樹脂片的硬化物的損耗正切極大時溫度、樹脂片的硬化物中的無機粒子的分散粒徑。將結果示於表1中。
(3)樹脂片向帶有凸塊的晶圓上的貼合步驟
於兩面具有剝離性基材的樹脂片向帶有凸塊的晶圓上的貼合是使用貼合裝置「VTM-200M」(商品名，高鳥(Takatori)(股)製造)來進行。
首先，自所述(2)中獲得的於兩面具有剝離性基材的樹脂片上將剝離性基材SR-3剝離，使樹脂片露出。繼而，於固定於貼合裝置台上且帶有平均高度為35μm的凸塊電極(448凸塊/晶片，間距60μm，周緣(peripheral)配置，金柱形凸塊)的半導體晶圓(直徑200mm，厚度625μm)的凸塊電極形成面上，以溫度80℃、貼合速度20mm/s，來貼合單面具有剝離性基材的樹脂片的不具有剝離性基材的面。利用切割器刃將半導體晶圓周圍的多餘樹脂片切斷，以凸塊電極埋沒於樹脂片中的狀態，獲得貼合有樹脂片的半導體晶圓。
(4)切割步驟
將所述(3)中獲得的貼合有樹脂片的半導體晶圓固定於帶框(tape frame)上。藉由使用晶圓貼片機(wafer mounter)裝置「FM-114」(商品名，科技視野(Technovision)(股)製造)，在與凸塊電極為相反側的晶圓基板面上貼合切割帶「UHP-110B」(商品名，東洋技術(Toyo Adtec)(股)製造)，來進行固定。繼而，自樹脂片上將剝離性基材SR-1剝離，使樹脂片露出。於切割裝置「DAD-3350」(商品名，迪思科(DISCO)(股)製造)的切削台上，以樹脂片面為上的方式將帶框固定，使用切割裝置的電荷耦合元件(charge coupled device，CCD)相機來進行對準。藉由切割裝置的自動對準功能，讀取半導體晶圓面的對準標記來進行對準。對準後，實施切割，獲得帶有樹脂片的半導體晶片(7.3mm見方)。
(5)倒裝晶片安裝
將所述(4)中製作的帶有樹脂片的半導體晶片，於電路基板(銅電極)上進行倒裝晶片安裝。安裝機是使用倒裝晶片黏合裝置「FC-2000」(商品名，東麗工程(Toray Engineering)(股)製造)。倒裝晶片黏合是以溫度為100℃、壓力為15N/晶片、時間為5秒的條件進行暫時壓接後，以溫度為200℃、壓力為100N/晶片的條件，且將時間設為10秒來進行正式壓接。藉此獲得半導體晶片與電路基板電性連接的半導體裝置。
安裝步驟後的樹脂片中所存在的氣泡的評價是藉由如下方式進行：藉由研磨而去除半導體晶片後，利用顯微鏡來觀察， 數出半導體裝置的半導體晶片與電路基板的黏接面(樹脂片)中所存在的氣泡的數量。評價基準如以下所述，將其結果示於表1中。
A：觀察到0個~5個的15μm以上大小的氣泡。
B：觀察到6個~20個的15μm以上大小的氣泡。
C：觀察到多於20個的15μm以上大小的氣泡。
(6)可靠性試驗
將所述(5)中製造的半導體裝置於85℃、60%RH的條件的恆溫恆濕槽中放置168小時，使其吸濕。然後，以260℃、5秒的回流條件進行加熱處理。繼而，將半導體裝置於-55℃下維持15分鐘，然後於125℃下維持15分鐘，將所述操作作為1個循環，將其進行1000個循環。
對進行所述處理後的半導體裝置的半導體晶片與基板間進行電性導通試驗(連接可靠性試驗)。將導通者評價為合格，將不導通者評價為不合格。使用10個樣品進行評價，記錄成為合格的樣品數(連接可靠性試驗A)。將結果示於表1中。
另外，將所述(5)中製造的半導體裝置於85℃、60%RH的恆溫高濕槽中放置168小時，使其吸濕後，以260℃、5秒的回流條件進行加熱處理後，將半導體裝置於-40℃下維持15分鐘，然後於125℃下維持15分鐘，將所述操作作為1個循環，將其進行1000個循環。
對進行所述處理後的半導體裝置的半導體晶片與基板間 進行電性導通試驗(連接可靠性試驗)。將導通者評價為合格，將不導通者評價為不合格。使用10個樣品進行評價，記錄成為合格的樣品數(連接可靠性試驗B)。將結果示於表1中。
實施例2~實施例46、比較例1~比較例2
除了以成為表1~表9所示組成比的方式將各成分進行調合以外，以與實施例1相同的方式進行樹脂片的製作以及評價。將結果示於表1~表9中。
實施例47
製作與實施例16同樣的樹脂片後，以250N/晶片來進行所述(5)倒裝晶片安裝步驟中的正式壓接的載重。其結果為，未出現半導體晶片的破損，氣泡的評價結果為A。進而，實施所述(6)可靠性試驗的結果為，連接可靠性試驗A及B的合格數均為10個。
比較例3
製作與比較例1同樣的樹脂片後，以250N/晶片來進行所述(5)倒裝晶片安裝步驟中的正式壓接的載重。其結果為，出現半導體晶片的破損，氣泡的評價結果為C。由於出現半導體晶片的破損，故而未實施所述(6)可靠性試驗。
[產業上之可利用性]
本發明的樹脂組成物可用作個人電腦以及行動終端機中使用的電子零件與印刷基板及可撓性基板的黏接、以及電子零件彼此的黏接或基板彼此的黏接時所使用的黏接劑。更詳細而言，可適宜用作當將IC、LSI等半導體晶片黏接於可撓性基板、玻璃環氧基板、玻璃基板、陶瓷基板等電路基板上時所使用的樹脂組成物。

Claims (5)

  1. 一種樹脂組成物，其含有(a)環氧化合物、(b)微膠囊型硬化促進劑、(c)無機粒子、以及(d)通式(1)所表示的化合物，且所述(a)環氧化合物為萘骨架環氧樹脂或者蒽骨架環氧樹脂，所述(c)無機粒子的分散粒徑為300nm以下，其中相對於所述(a)環氧化合物100重量份，所述(b)微膠囊型硬化促進劑的含量為0.1重量份~50重量份；相對於所述樹脂組成物中的固體成分，所述(c)無機粒子的含量為40重量%~70重量%；以及相對於所述樹脂組成物的包含溶劑的總量，所述(d)通式(1)所表示的化合物的含量，為0.1重量%~10重量%； (所述通式(1)中，r、s及t分別表示0~2的整數)。
  2. 如申請專利範圍第1項所述的樹脂組成物，其中所述(d)通式(1)所表示的化合物為乙醯丙酮。
  3. 一種樹脂片的製造方法，其將如申請專利範圍第1項或第2項所述的樹脂組成物塗佈於剝離性基材上後，將揮發成分去除。
  4. 一種半導體裝置的製造方法，其藉由在第一電路構件與第二電路構件之間介隔利用如申請專利範圍第3項所述的樹脂片的製造方法來獲得的樹脂片，藉由進行加熱加壓，使所述第一電路 構件與所述第二電路構件電性連接。
  5. 一種半導體裝置的製造方法，其中於如申請專利範圍第4項所述的半導體裝置的製造方法中，加熱加壓時的壓力為200N~500N。
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