TWI673318B - 環氧樹脂組成物、半導體密封劑及半導體裝置 - Google Patents

環氧樹脂組成物、半導體密封劑及半導體裝置 Download PDF

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TWI673318B
TWI673318B TW103141185A TW103141185A TWI673318B TW I673318 B TWI673318 B TW I673318B TW 103141185 A TW103141185 A TW 103141185A TW 103141185 A TW103141185 A TW 103141185A TW I673318 B TWI673318 B TW I673318B
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component
epoxy resin
resin composition
semiconductor
butadiene
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TW103141185A
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TW201527410A (zh
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山澤朋也
小原和之
小越弘大
阿部信幸
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日商納美仕股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
    • C08G59/22—Di-epoxy compounds
    • C08G59/24—Di-epoxy compounds carbocyclic
    • C08G59/245—Di-epoxy compounds carbocyclic aromatic
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
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    • C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
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Abstract

本發明係提供一種環氧樹脂組成物，其特徵為具有(A)環氧樹脂、(B)硬化劑、(C)0.1~10質量%之平均粒徑10nm以上且100nm以下的二氧化矽填料、(D)47~75質量%之平均粒徑0.3μm以上且2μm以下的二氧化矽填料、(E)0.1~8質量%之彈性體，且包含合計為50.1~77質量%之前述(C)成分及前述(D)成分。

Description

環氧樹脂組成物、半導體密封劑及半導體裝置
本發明係關於環氧樹脂組成物、半導體密封劑、及半導體裝置。
將半導體晶片(半導體元件)實裝於配線基板之技術係倒裝晶片實裝。倒裝晶片實裝係於半導體晶片之表面藉由形成突起狀電極(凸塊)，使此表面面對配線基板直接連接之實裝方法。為了保護連接之半導體晶片及配線基板、及凸塊，被稱為底部填充劑之密封樹脂填充於半導體晶片與配線基板之間。
底部填充劑中主要係使用環氧樹脂。環氧樹脂、半導體晶片、及配線基板分別具有不同線膨脹係數。因此，連接部無法吸收應力時，有時於該連接部發生破裂。為了抑制破裂的發生，底部填充劑中，使二氧化矽等之線膨脹係數比較小之填料分散。
然而，近年來，倒裝晶片實裝中，已變成使用藉由金屬柱之凸塊。例如銅柱凸塊與以往之焊錫凸塊比較，具有如以下之各種優勢。亦即，由於銅柱凸塊可縮小 凸塊的間距，故可減低鉛的使用量，對環境造成的影響小，且由於熱傳導性高故放熱特性優異，進而由於電氣傳導度高可減低寄生電阻。惟，使用金屬柱凸塊時，有時分離底部填充劑中之填料。此被認為係藉由用在柱之金屬、與用在焊錫之金屬之間所產生的電位差，並藉由將底部填充劑中遷移填料，而產生填料的分離。
因此，正研究抑制在底部填充劑之填料的分 離之(促使填料的分散)技術。專利文獻1中，金屬柱之表面係以焊錫被膜。據此，揭示有電子零件的實裝方法，其係促進底部填充劑中之填料的分散，且提昇倒裝晶片實裝之連接信賴性。
本發明係提供促進填料的分散之樹脂組成物。根據本發明之樹脂組成物，例如如將金屬柱之表面以焊錫被膜並不需要使用特別之步驟。
本發明之環氧樹脂組成物，其特徵為包含(A)環氧樹脂、(B)硬化劑、(C)0.1~10質量%之平均粒徑10nm以上且100nm以下的二氧化矽填料、(D)47~75質量%之平均粒徑0.3μm以上且2μm以下的二氧化矽填料、(E)0.1~8質量%之彈性體，且包含合計為50.1~77質量%之前述(C)成分及前述(D)成分。
前述(C)成分及前述(D)成分當中之至少一者可為以矽烷偶合劑進行表面處理。
前述(D)成分可藉由下述式(1)所示之構造式表 示之胺基矽烷來進行表面處理。
相對於前述(A)成分之環氧基1當量，前述(B)成分可包含0.5當量以上且1.8當量以下。
前述(B)成分可為酸酐硬化劑、酚樹脂硬化劑、或胺硬化劑。
前述(A)成分可包含雙酚F型環氧樹脂、雙酚A型環氧樹脂、萘型環氧樹脂、胺基酚型環氧樹脂當中之至少一個。
又，上述之態樣中，前述(E)成分可包含丁二烯系彈性體、矽氧烷系彈性體、丙烯醯基共聚物、苯乙烯丁二烯系彈性體、丁二烯‧丙烯腈‧2,3-環氧丙基甲基丙烯酸酯‧二乙烯基苯共聚合物、丁二烯‧丙烯腈‧甲基丙烯酸‧二乙烯基苯共聚合物、胺基末端丁二烯‧丙烯腈共聚合物、及羧基末端丁二烯‧丙烯腈共聚合物當中之至少一個。
此樹脂組成物可藉由於前述(A)成分之至少一部分混合前述(C)成分生成母料，於該母料混合其他成分來製造。
又，本發明係提供一種使用上述之環氧樹脂組成物之半導體密封劑。
上述半導體密封劑可密封藉由2種以上之金 屬或合金所形成之半導體裝置的導通部分。
前述2種以上之金屬或合金可為選自Au、 Ag、Cu、Sn、Pb、Ni、Pd、Co、Cd、Bi、In、Sb、及Zn中之2種以上之金屬或可為將該金屬作為基之合金。
所密封之前述半導體裝置的導通部分為2種 之金屬或合金，將密封前述導通部分之前述環氧樹脂組成物的剖面，根據前述2種之金屬或合金之間的邊界，畫分成2個區域，使用在該各區域之前述(C)成分及前述(D)成分的占有率，藉由以下之式所算出之填料分散指數可為50以上且150以下。
填料分散指數=100×(區域Ra的占有率)/(區域Rb的占有率)
進而，本發明係提供一種使用上述之半導體密封劑之半導體裝置。
藉由本發明可促進填料的分散。
1‧‧‧配線基板
10‧‧‧底部填充劑
2‧‧‧電極端子
3‧‧‧絕緣膜
4‧‧‧焊錫
5‧‧‧晶片基板
7‧‧‧電極端子
8‧‧‧銅柱
9‧‧‧鈍化
L‧‧‧邊界線
圖1係用以說明填料之分散指數評價之圖。
圖2係擴大圖1所示區域II之圖。
本發明之環氧樹脂組成物係包含(A)環氧樹 脂、(B)硬化劑、(C)小徑二氧化矽填料、(D)大徑二氧化矽填料、及(E)彈性體。
作為(A)成分之例，可列舉雙酚F型環氧樹 脂、雙酚A型環氧樹脂、萘型環氧樹脂、胺基酚型環氧樹脂、酚酚醛清漆型環氧樹脂、脂環式環氧樹脂、矽氧烷型環氧樹脂、聯苯型環氧樹脂、環氧丙基酯型環氧樹脂、環氧丙基胺型環氧樹脂、乙內醯脲型環氧樹脂、及萘環含有環氧樹脂。環氧樹脂組成物中，於此所例示之化合物可單獨使用，亦可混合2個以上使用。
作為(B)成分之例，可列舉酸酐系硬化劑、酚 樹脂系硬化劑、及胺系硬化劑。(B)成分相對於(A)成分之環氧基1當量，以包含0.5當量以上且1.8當量以下為佳。
作為(C)成分及(D)成分之例，可列舉非晶質二 氧化矽、結晶性二氧化矽、熔解二氧化矽、粉碎二氧化矽、及奈米二氧化矽。(C)成分及(D)成分的形狀，並未特別限定，可為粒狀、粉末狀、及鱗片等之任一形態。而且，所謂在本發明之二氧化矽填料之平均粒徑，係指無論二氧化矽填料的形狀，藉由雷射繞射法或電界放射型掃描電子顯微鏡(FE-SEM)所測定之體積基準之D50(中值粒徑)。
(C)成分之平均粒徑以10nm以上且100nm以 下為佳。(D)成分之平均粒徑以0.3μm以上且2μm以下為 佳。本發明之環氧樹脂組成物以包含0.1質量%以上且10質量%以下之(C)成分，且包含47質量%以上且75質量%以下之(D)成分為佳。進而，本發明之環氧樹脂組成物包含合計為50.1質量%以上且77質量%以下之(C)成分及(D)成分為佳。更佳為(C)成分與(D)成分的合計範圍為52質量%以上且77質量%以下的範圍。
尚，(C)成分及(D)成分當中之至少一者可為以 矽烷偶合劑進行表面處理。作為表面處理所使用之矽烷偶合劑，可列舉環氧系、甲基丙烯基系、胺基系、乙烯基系、環氧丙氧基系、及巰基系等各種之矽烷偶合劑。其中，(D)成分之表面處理中，以使用以下式(1)所示構造之胺基矽烷為佳。
作為(E)成分之例，可列舉丁二烯系彈性體、 矽氧烷系彈性體、丙烯醯基共聚物、苯乙烯丁二烯系彈性體、丁二烯‧丙烯腈‧2,3-環氧丙基甲基丙烯酸酯‧二乙烯基苯共聚合物、丁二烯‧丙烯腈‧甲基丙烯酸‧二乙烯基苯共聚合物、胺基末端丁二烯‧丙烯腈共聚合物、及羧基末端丁二烯‧丙烯腈共聚合物。作為(E)成分，於此所例示之化合物可單獨使用，亦可混合2個以上之化合物使用。即(E)成分若為包含上述之化合物當中之至少一個之 彈性體即可。(E)成分以包含0.1質量%以上且8質量%以下為佳。
環氧樹脂組成物除了(A)、(B)、(C)、(D)、及 (E)成分，可包含離子分離器劑、顏料、染料、消泡劑、應力緩和劑、pH調整劑、促進劑、界面活性劑、及偶合劑等之添加劑。
環氧樹脂組成物可將半導體元件等之電子裝 置作為倒裝晶片實裝或BGA(Ball Grid Array)/CSP(Chip Size Package)實裝時之半導體密封劑(底部填充劑)使用。 此環氧樹脂組成物亦可將電子裝置作為與基板或封裝接著時之接著劑使用。
倒裝晶片實裝或BGA/CSP實裝時，首先接 合半導體元件與基板(或封裝)。其次，於半導體元件與基板之隙間注入半導體密封劑。具體而言，係沿著半導體元件之外周圍塗佈半導體密封劑。半導體密封劑係藉由毛細現象而擴散於間隙內。據此，半導體密封劑係以進行此製程之溫度為液狀較佳。所注入之半導體密封劑係由加熱(例如80~165℃)進行熱硬化。
圖1係例示使用本發明之半導體密封劑進行 密封之半導體裝置之圖。圖1中，顯示使用金屬柱之倒裝晶片實裝之例。尚，圖1係顯示半導體裝置之剖面。
於基板1之上形成電極2。於電極2以外之處 形成絕緣膜3。於電極2之上配置有焊錫凸塊4。又，於半導體晶片5之上(於圖係面向下)形成電極7。半導體晶 片5整體係以鈍化9被覆。相當於電極7之位置中設置開口。於電極7之上形成金屬柱一種之銅柱8。
銅柱8係以銅(Cu)或銅作為主體之合金來形 成。焊錫凸塊4係以錫(Sn)作為主體之合金來形成。尚，焊錫凸塊及金屬柱之材料並不限於此所例示者。焊錫凸塊及金屬柱，例如係藉由選自Au、Ag、Cu、Sn、Pb、Ni、Pd、Co、Cd、Bi、In、Sb、及Zn之2種以上之金屬、或將其金屬作為基之合金來形成。如此，本實施形態之半導體密封劑係用在導通部分藉由2種以上之金屬、或將其金屬作為基之合金所形成之半導體裝置的導通部分之密封。
環氧樹脂組成物，例如同時或分別將(A)成分 ~(E)成分及其他添加劑等藉由必要一邊加入加熱處理，一邊進行攪拌、熔解、混合、或分散來製造。此等之混合、攪拌、及分散等之方法並未特別限定。可使用具備攪拌及加熱裝置之軋碎機、3本輥磨粉機、球磨機、行星式混合機、或珠粒磨粉機等。又，可組合此等裝置使用。於此，可藉由混合(A)成分與(C)成分，來調製母料。可藉由混合所得之母料與其他成分，來製造環氧樹脂組成物。
[實施例] (1)環氧樹脂組成物之調製
表1~10係表示於實施例1~37及比較例1~9，作為密封劑所使用之環氧樹脂組成物的組成。又，此等之表 亦表示後述作為密封劑之環氧樹脂組成物的評價結果。表1~10中，環氧樹脂組成物的組成排除等量比係以質量份(相當於質量份的合計為100之質量%)表示。
作為表中之(A)成分，係使用環氧樹脂a1~a5 當中之至少一個。作為環氧樹脂a1，係使用雙酚F型環氧樹脂一種之新日鐵住金化學股份有限公司製之YDF8170。作為環氧樹脂a2，係使用雙酚A型環氧樹脂一種之DIC股份有限公司製之850CRP。作為環氧樹脂a3，係使用萘型環氧樹脂一種之DIC股份有限公司製之HP-4032D。作為環氧樹脂a4，係使用胺基酚型環氧樹脂一種之三菱化學股份有限公司製之jer630。作為環氧樹脂a5，係使用環狀脂肪族型環氧樹脂一種之新日鐵住金化學股份有限公司製之ZX1658GS。
作為表中之(B)成分，係使用硬化劑b1~b5 當中之至少一個。作為硬化劑b1，係使用胺硬化劑之日本化藥股份有限公司製之KAYAHARDAA。作為硬化劑b2，係使用胺硬化劑之ADEKA股份有限公司製之EH105L。作為硬化劑b3，係使用胺硬化劑之雅寶(Albermarle)公司製之ETHACURE100。作為硬化劑b4，係使用酸酐硬化劑之三菱化學股份有限公司製之YH307。 作為硬化劑b5，係使用酚樹脂硬化劑之明和化成股份有限公司製之MEH-8005。
作為表中之(C)成分，係使用Admatechs股份 有限公司製之YA010C(平均粒徑：10nm)、YA050C(平均 粒徑：50nm)、及YC100C(平均粒徑：100nm)當中之任一種。上述填料之平均粒徑為中值粒徑(D50)。又，此平均粒徑係藉由電界放射型掃描電子顯微鏡(FE-SEM)所測定之值。
作為表中之(D)成分，係使用宇部Ekushimo 股份有限公司製之Hipresica 0.2μm(平均粒徑：0.2μm)、Admatechs股份有限公司製之SE-1050(平均粒徑：0.3μm)、SE-2300(平均粒徑：0.6μm)、SE-4050(平均粒徑：1μm)、及SE-6050(平均粒徑：2μm)當中之任一種。 上述平均粒徑為中值粒徑(D50)。又，此平均粒徑係藉由雷射繞射散射式粒度分布計所測定之值。
作為上述(D)成分之表面處理劑，係使用表面 處理劑f1~f3當中之任一種。作為表面處理劑f1，係使用信越化學工業股份有限公司製之KBM403(3-環氧丙氧基丙基三甲氧基矽烷)。作為表面處理劑f2，係使用信越化學工業股份有限公司製之KBM503(3-甲基丙烯醯氧基丙基三甲氧基矽烷)。作為表面處理劑f3，係使用信越化學工業股份有限公司製之KBE9103(3-三乙氧基矽烷基-N-(1,3-二甲基-亞丁基)丙基胺、式(1)之化合物)。
作為表中之(E)成分，係使用彈性體e1~e9當 中之至少一個。作為彈性體e1，係使用丁二烯系彈性體一種之Kaneka股份有限公司製之MX137。作為彈性體e2，係使用矽氧烷系彈性體一種之Kaneka股份有限公司製之MX965。作為彈性體e3，係使用苯乙烯丁二烯系彈 性體一種之Kaneka股份有限公司之MX135。作為彈性體e4，係使用丙烯醯基共聚物一種之ARKEMA股份有限公司製之M52N。作為彈性體e5，係使用丁二烯‧丙烯腈‧2,3環氧丙基甲基丙烯酸酯‧二乙烯基苯共聚合物一種之JSR股份有限公司製之XER-81。作為彈性體e6，係使用丁二烯‧丙烯腈‧甲基丙烯酸‧二乙烯基苯共聚合物一種之JSR股份有限公司製之XER-91。作為彈性體e7，係使用胺基末端丁二烯‧丙烯腈共聚合物一種之宇部興產股份有限公司製之ATBN。作為彈性體e8，係使用羧基末端丁二烯‧丙烯腈共聚合物一種之宇部興產股份有限公司製之CTBN。作為彈性體e9，係使用矽氧烷系彈性體一種之信越矽氧烷股份有限公司製之KMP-605。
除了上述(A)~(E)成分之外，作為硬化促進劑 係使用四國化成股份有限公司製之2P4MZ。
(2)評價
將實施例1~37及比較例1~9所使用之環氧樹脂組成物作為樣品，進行以下之評價。
(2-1)分散指數之評價
圖2係例示半導體裝置之剖面照片之圖。此圖係於圖1以「II」表示之區域(區域II)的剖面照片。圖1之區域II中，流入挾住配線基板1、晶片基板5、銅柱8、及焊錫4之空間後，包含硬化之底部填充劑10的剖面。將此 區域II使用掃描型電子顯微鏡(SEM)等攝影。將其攝影圖像藉由圖像處理軟體，如以下般由電腦來分析。亦即，首先，此攝影圖像當中，底部填充劑10之區域係藉由用戶等來指定。將被指定之該區域之亮度分布的中央值作為基準，來進行二值化處理。於此，二值化之圖像當中，白色部分係顯示填料，黑色部分係顯示填料以外之樹脂成分。 其次，指定之區域係將銅柱8與焊錫4之邊界線L的延長線作為邊界，畫分成銅柱8側之區域Ra、及焊錫4側之區域Rb2個。而且根據銅柱8側之區域Ra、及焊錫4側之區域Rb的各圖像，算出個別區域中之二氧化矽填料的占有率。分散指數係藉由以下式來算出。
分散指數=100×(區域Ra的占有率)/(區域Rb的占有率)
分散指數係表示以100時之各區域分布均勻 填料。分散指數小於100時，顯示填料偏向區域Rb。分散指數小時顯示填料大幅偏向區域Rb。分散指數顯示增大越接近100時，填料之分布越接近更均勻之狀態。於此，分散指數為50以下時，其樣品之填料分布的均勻性判斷為不良。尚，圖像處理中，係使用美國國立衛生研究所(NIH：National Institutes of Health)之Image J。
(2-2)黏度之評價
使用Brookfield旋轉黏度計，以50rpm，測定在25℃ 之上述環氧樹脂組成物的黏度。
(2-3)TI(觸變指數(Thixotropic index))值
以5rpm及50rpm測定上述環氧樹脂組成物的黏度。將所測定之在5rpm的黏度之值除以在50rpm的黏度之值的值作為TI值。
(2-4)注入性之評價
110℃中，於20μm之間隙(Gap)注入評價用樣品。測定注入之評價用樣品從入口至到達20mm位置為止的時間。顯示到達為止的時間越短注入性越良好。尚，表中的注入性之欄有「-」之記載，係意指評價用樣品未到達至20mm位置(亦即不良)。
(2-5)接著強度之評價
於FR-4上裝填約0.5mg之評價用樣品。於其上載放2mm平方矽晶片，於室溫放置5分鐘。隨後，使用送風乾燥機，以150℃下120分鐘之條件，硬化評價用樣品。對於如此進行所得之試片，將接著強度使用桌上型強度測定機(Aikoh engineering(股)製1605HTP)測定。尚，將藉由10次測定所得之測定值的平均值作為檢查值。
(3)評價結果 (3-1)對於彈性體量
表1係表示實施例1~5、以及比較例1及2之環氧樹脂組成物之組成、以及評價的結果。以下，表中，環氧樹脂組成物的組成係以質量份(質量%)表示。表1係顯示(E)成分的含量變化之例。於亦未包含(C)成分及(E)成分當中之任一種之比較例1，分散指數為38。另外，於包含(C)成分及(E)成分之實施例1~5，分散指數成為50以上。(E)成分的含量增加時，分散指數接近100。亦即，(E)成分的含量增加時，改善填料分布的均勻性。惟，(E)成分的含量成為8.3質量%(比較例2)時，於注入性實驗發生不良。
(3-2)對於彈性體之種類
表2係表示實施例3及6~13之環氧樹脂組成物之組成、以及評價的結果。表2係顯示(E)成分之種類變化之例。作為(E)成分即使使用彈性體e1~e9之任一種，亦可改善填料分布之均勻性。
(3-3)對於小徑二氧化矽填料的量
表3係表示實施例3及14~16、以及比較例3及4之環氧樹脂組成物的組成、以及評價的結果。表3係顯示(C)成分的含量變化之例。(C)成分的含量為0.05質量%(比較例3)時，分散指數為44，填料分布之均勻性為不良。 (C)成分的含量增加時，分散指數接近為100，改善填料分布之均勻性。據此，(C)成分的含量以0.1質量%以上為佳。惟，(C)成分的含量成為11質量%時，黏度成為132Pa‧s。據此，從作為密封劑之適當黏度的觀點來看，(C)成分的含量以10質量%以下為佳。
(3-4)對於小徑二氧化矽填料之平均粒徑
表4係表示實施例3、17、18及比較例5之環氧樹脂組成物的組成、以及評價的結果。表4係顯示(C)成分之平均粒徑變化之例。尚，比較例5中，取代(C)成分改使用平均粒徑0.2μm(亦即200nm)之(D)成分。未包含(C)成分時(比較例5)，以分散指數發生不良。包含(C)成分時，改善分散指數。此時，(C)成分之平均粒徑越小，越能改善分散指數。亦即，(C)成分之平均粒徑於10~100nm的範圍，改善分散指數。
(3-5)對於大徑二氧化矽填料之平均粒徑
表5係表示實施例3、19、20及比較例6之環氧樹脂組成物的組成、以及評價的結果。表5係顯示(D)成分之平均粒徑變化之例。(D)成分之平均粒徑於0.2~2μm的範圍，於分散指數實驗未觀測到不良。隨著(D)成分之平均粒徑變小改善分散指數。相反黏度惡化。(D)成分之平均粒徑為0.2μm(比較例6)時，顯示195Pa‧s之高黏度。據此，從作為密封劑之適當之黏度的觀點來看，(D)成分之平均粒徑以0.3μm以上為佳。
(3-6)對於大徑二氧化矽填料的量
表6係表示實施例3、21~24及比較例7~9之環氧樹脂組成物的組成、以及評價的結果。表6係顯示(D)成分的含量變化之例。(D)成分的含量於52~75質量%的範圍改善分散指數。惟，(D)成分的含量越多時注入性越惡化。尤其是(D)成分的含量成為76質量%(比較例9)時，於注入性實驗觀測到不良。據此，從作為密封劑之適度之注入性的觀點來看，(D)成分的含量以75%以下為佳。尚，確認(C)成分的含量與(D)成分的含量的合計少於50.1質量%時(比較例7及8)，環氧樹脂組成物之分散指數的值變小於50。
(3-7)對於大徑二氧化矽填料之表面處理
表7係表示實施例3及25~27之環氧樹脂組成物的組成、以及評價的結果。表7係顯示(D)成分之表面處理變化之例。即使使用(D)成分為具有環氧基、甲基丙烯酸基、及胺基當中之任一種之矽烷偶合劑來進行表面處理，又，即使未進行表面處理，於分散指數實驗未發生不良。
(3-8)對於硬化劑之當量比
表8係表示實施例3、28及29之環氧樹脂組成物的組成、以及評價的結果。表8係顯示對於(A)成分之(B)成分的當量比變化之例。相對於(A)成分之環氧基1當量之(B)成分的當量比於0.5當量以上且1.8當量以下的範圍，於分散指數實驗未發生不良。
(3-9)對於環氧樹脂之種類
表9係表示實施例3及30~33之環氧樹脂組成物的組成、以及評價的結果。表9係顯示(A)成分之種類、及(A)成分與(B)成分的含有比變化之例。(A)成分即使為環氧樹脂a1~a5當中之任一種，於分散指數實驗並未觀測到不良。
(3-10)對於硬化劑的種類
表10係表示實施例3、及實施例34~37之環氧樹脂組成物的組成、以及評價的結。表10係顯示(B)成分之種類、及(A)成分與(B)成分的含有比變化之例。(B)成分即使為硬化劑b1~b5當中之任一種，於分散指數實驗並未發生不良。
進而，本發明之環氧樹脂組成物可為以下之第1至8之環氧樹脂組成物。
上述第1之環氧樹脂組成物，係一種環氧樹脂組成物，其特徵為具有(A)環氧樹脂、(B)硬化劑、(C)0.1~10質量%之平均粒徑10nm以上且100nm以下的二氧化矽填料、(D)47~75質量%之平均粒徑0.3μm以上且2μm以下的二氧化矽填料、(E)0.1~8質量%之彈性體，且包含合計為47.1~77質量%之前述(C)成分及前述(D)成分。
上述第2之環氧樹脂組成物，係如上述第1之環氧樹脂組成物，其中，上述(C)成分及上述(D)成分之至少一個為以矽烷偶合劑進行表面處理。
上述第3之環氧樹脂組成物，係如上述第1或2之環氧樹脂組成物，其中上述(D)成分為以下式(1)所示構造之胺基矽烷進行表面處理，
上述第4之環氧樹脂組成物，係如上述第1至3中任一項之環氧樹脂組成物，其中，相對於上述(A)成分之環氧基1當量，包含0.5~1.8當量之上述(B)成分。
上述第5之環氧樹脂組成物，係如上述第1至4中任一項之環氧樹脂組成物，其中，前述(B)成分為酸酐硬化劑、酚樹脂硬化劑、或胺硬化劑。
上述第6之環氧樹脂組成物，係如上述第1至5中任 一項之環氧樹脂組成物，其中，前述(A)成分係包含雙酚F型環氧樹脂、雙酚A型環氧樹脂、萘型環氧樹脂、胺基酚型環氧樹脂之至少一個。
上述第7之環氧樹脂組成物，係如上述第1至6中任一項之環氧樹脂組成物，其中，上述(E)成分係包含丁二烯系彈性體、矽氧烷系彈性體、丙烯醯基共聚物、苯乙烯丁二烯系彈性體、丁二烯‧丙烯腈‧2,3-環氧丙基=甲基丙烯酸酯‧二乙烯基苯共聚合物、丁二烯‧丙烯腈‧甲基丙烯酸‧二乙烯基苯共聚合物、胺基末端丁二烯‧丙烯腈共聚物、羧基末端丁二烯‧丙烯腈共聚物之至少一個。
上述第8之環氧樹脂組成物，係如上述第1至7中任一項之環氧樹脂組成物，其中，藉由於上述(A)環氧樹脂之至少一部分混合上述(C)平均粒徑10~100nm之二氧化矽填料，而生成母料，於該母料混合其他成分而製造。
進而，本發明之半導體密封劑可為以下之第1至4之半導體密封劑。
上述第1之半導體密封劑係使用上述第1至8中任一項之環氧樹脂組成物之半導體密封劑。
上述第2之半導體密封劑，係如上述第1之半導體密封劑，其中，密封之前述半導體裝置的導通部分為2種以上之金屬或合金。
上述第3之半導體密封劑，係如上述第2之半導體密封劑，其中，密封之前述半導體裝置的導通部分係藉由選自Au、Ag、Cu、Sn、Pb、Ni、Pd、Co、Cd、Bi、In、 Sb、Zn之2種以上之金屬或將該金屬作為基之合金而形成。
上述第4之半導體密封劑，係如上述第1之半導體密封劑，其中，所密封之前述半導體裝置的導通部分為2種之金屬或合金，將密封前述導通部分之前述環氧樹脂組成物的剖面，沿著前述2種之金屬或合金之邊界來畫分成2個區域，因應在該各區域之前述(C)成分及前述(D)成分之面積的比所算出之填料分散指數為50以上且150以下。
進而，本發明之半導體裝置係使用如上述第1至4中任一項之半導體密封劑之半導體裝置。

Claims (11)

  1. 一種環氧樹脂組成物，其特徵為包含(A)環氧樹脂、與(B)硬化劑、與(C)0.1~10質量%之平均粒徑10nm以上且100nm以下的二氧化矽填料、與(D)47~75質量%之平均粒徑0.3μm以上且2μm以下的二氧化矽填料、與(E)0.1~8質量%之彈性體，且包含合計為50.1~77質量%之前述(C)成分及前述(D)成分，前述(D)成分係藉由以下式(1)之構造式表示之胺基矽烷來進行表面處理，
    Figure TWI673318B_C0001
  2. 如請求項1之環氧樹脂組成物，其中，相對於前述(A)成分之環氧基1當量，係包含前述(B)成分0.5~1.8當量。
  3. 如請求項1或2之環氧樹脂組成物，其中，前述(B)成分為酸酐硬化劑、酚樹脂硬化劑、或胺硬化劑。
  4. 如請求項1或2之環氧樹脂組成物，其中，前述(A)成分係包含雙酚F型環氧樹脂、雙酚A型環氧樹脂、萘型環氧樹脂、胺基酚型環氧樹脂當中之至少一個。
  5. 如請求項1或2之環氧樹脂組成物，其中，前述(E)成分係包含丁二烯系彈性體、矽氧烷系彈性體、丙烯醯基共聚物、苯乙烯丁二烯系彈性體、丁二烯‧丙烯腈‧2,3-環氧丙基甲基丙烯酸酯‧二乙烯基苯共聚合物、丁二烯‧丙烯腈‧甲基丙烯酸‧二乙烯基苯共聚合物、胺基末端丁二烯‧丙烯腈共聚合物、及羧基末端丁二烯‧丙烯腈共聚合物當中之至少一個。
  6. 如請求項1或2之環氧樹脂組成物，其中，藉由於前述(A)成分之至少一部分混合前述(C)成分，而生成母料，於該母料混合其他成分而製造。
  7. 一種半導體密封劑，其係使用如請求項1~6中任一項之環氧樹脂組成物。
  8. 如請求項7之半導體密封劑，其係密封藉由2種以上之金屬或合金所形成之半導體裝置的導通部分。
  9. 如請求項8之半導體密封劑，其係前述2種以上之金屬或合金係選自Au、Ag、Cu、Sn、Pb、Ni、Pd、Co、Cd、Bi、In、Sb、及Zn當中之2種以上之金屬或將該金屬作為基之合金。
  10. 如請求項8之半導體密封劑，其係所密封之前述半導體裝置的導通部分為2種之金屬或合金，將密封前述導通部分之前述環氧樹脂組成物的剖面，根據前述2種之金屬或合金之間的邊界，畫分成區域Ra及區域Rb之2個區域，使用在該各區域之前述(C)成分及前述(D)成分的占有率，藉由以下之式所算出之填料分散指數為50以上且150以下，填料分散指數=100×(區域Ra的占有率)/(區域Rb的占有率)。
  11. 一種半導體裝置，其係使用如請求項7~10中任一項之半導體密封劑。
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