TW201609946A - 環氧樹脂組成物、樹脂片、預浸體及覆金屬積層板、印刷配線基板、半導體裝置 - Google Patents
環氧樹脂組成物、樹脂片、預浸體及覆金屬積層板、印刷配線基板、半導體裝置 Download PDFInfo
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- TW201609946A TW201609946A TW104124878A TW104124878A TW201609946A TW 201609946 A TW201609946 A TW 201609946A TW 104124878 A TW104124878 A TW 104124878A TW 104124878 A TW104124878 A TW 104124878A TW 201609946 A TW201609946 A TW 201609946A
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- Prior art keywords
- epoxy resin
- resin composition
- prepreg
- metal
- glass
- Prior art date
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
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Abstract
本發明之目的在於提供一種環氧樹脂組成物、及使用其之樹脂片、覆金屬積層板、印刷配線基板、以及半導體裝置,該環氧樹脂組成物之硬化物為高耐熱性且吸水性、介電常數低。本發明之環氧樹脂組成物係以下述通式(1)所示之環氧樹脂與胺系硬化劑為必須成分。
□(式中,(a)(b)之比率為(a)/(b)=1~3;G表示環氧丙基;n為重複數,為0~5)
Description
本發明係關於一種提供耐熱性與耐水性優異之硬化物之環氧樹脂組成物、使其含浸於纖維基材而成之預浸體、樹脂片、覆金屬積層板、印刷配線基板、及半導體裝置。
環氧樹脂組成物由於作業性及其硬化物之優異電氣特性、耐熱性、接著性、耐濕性(耐水性)等而廣泛用於電氣/電子零件、結構用材料、接著劑、塗料等領域中。
但是近年來,於電氣/電子領域中,隨著其發展,要求以樹脂組成物之高純度化為首之耐濕性、密接性、介電特性、用以使填充劑(無機或有機填充劑)高填充之低黏度化、用以使成型週期變短之反應性提高等各種特性之進一步提昇。又,作為結構材料,於航空航天材料、娛樂/運動器具用途等中要求輕量且機械物性優異之材料。尤其於半導體密封領域、基板(基板自身或其周邊材料)中,該要求特性逐年提高,例如要求由半導體之驅動溫度上升而引起之周邊材料之高Tg化等。
通常若環氧樹脂高Tg化,則吸水率上升(非專利文獻1)。
此係因交聯密度提高所產生之影響。然而,於對要求低吸濕之半導體周邊材料要求高Tg化中,具有該相反特性之樹脂的開發係當務之急。
另一方面,於專利文獻1中揭示有具有聯苯骨架之酚系酚醛清漆樹脂及藉由將其環氧化而獲得之酚系酚醛清漆型環氧樹脂,且記載有對半導體密封劑用途之有用性。
然而,本環氧樹脂係以與酚樹脂之組合而兼顧高耐熱性與難燃性,但吸水率高,於用於需要非常高可靠性之電子材料用時存在問題。
又,關於含有該等環氧樹脂與胺系硬化劑之組成物之特性,並無任何記載,又,關於印刷配線基板用途之有用性,亦無記載。
專利文獻1:日本特開2013-43958號公報
非專利文獻1:小椋一郎,「環氧樹脂之化學結構與特性之關係」,DIC Technical Review No.7,日本,2001年,第7頁
本發明係為了解決此種問題進行研究而結果產生者,其課題在於提供一種環氧樹脂組成物、及使用其之預浸體、樹脂片、覆金屬積層板、印刷配線基板、以及半導體裝置,該環氧樹脂組成物之硬化物為高耐熱性且吸水性、介電係數低。
本發明者等人為了解決上述問題而進行努力研究,結果完成本發明。
即,本發明係提供:(1)一種環氧樹脂組成物,其以下述通式(1)所示之環氧樹脂與胺系硬化劑為必須成分,
(式中,(a)(b)之比率為(a)/(b)=1~3;G表示環氧丙基;n為重複數,為0~5);(2)一種預浸體,其係將上述(1)所記載之環氧樹脂組成物含浸於纖維基材而成;(3)如上述(2)所記載之預浸體,其中上述纖維基材為玻璃纖維基材;(4)如上述(3)所記載之預浸體,其中上述玻璃纖維基材包含選自由T玻璃、S玻璃、E玻璃、NE玻璃、及石英玻璃組成之群中之至少1種;(5)一種覆金屬積層板,其於上述(2)至(4)中任一項所記載之預浸體之至少一面積層有金屬箔;
(6)一種樹脂片,其係將由上述(1)所記載之環氧樹脂組成物構成之絕緣層形成於膜上、或金屬箔上而成;(7)一種印刷配線基板,其係將上述(5)所記載之覆金屬積層板用於內層電路基板而成;(8)一種印刷配線基板,其係使上述(2)至(4)中任一項所記載之預浸體或上述(6)所記載之樹脂片硬化而成;(9)一種半導體裝置,其係於上述(7)或(8)所記載之印刷配線基板上搭載半導體元件而成。
本發明之環氧樹脂組成物提供關於其硬化物可同時達成高耐熱性與耐水性之硬化物,因此為對製作印刷配線基板或增層基板等積層板極有用之材料。
根據本發明,可提供一種環氧樹脂組成物及使用其之預浸體、樹脂片、覆金屬積層板、印刷配線基板,以及半導體裝置,上述環氧樹脂組成物之硬化物為高耐熱性且吸水性、介電常數低。
圖1係表示環氧樹脂組成物之硬化物的耐熱性與吸水特性
之關係的圖表。
以下,對本發明之環氧樹脂組成物進行說明。
本發明之環氧樹脂組成物係以作為環氧樹脂之下述式(1)所示之化合物(以下,稱為「式(1)之環氧樹脂」)與胺系硬化劑為必須成分。
(式中,(a)(b)之比率為(a)/(b)=1~3;G表示環氧丙基;n為重複數,為0~5)。
本發明中所使用之式(1)之環氧樹脂可利用日本特開2011-252037號公報、日本特開2008-156553號公報、日本特開2013-043958公報、國際公開WO2012/053522、WO2007/007827所記載之方法進行合成,但若具有上述式(1)之結構,則亦可使用任意方法。
其中,於本發明中,尤其是使用上述式(a)與上述式(b)之比例(多官能化率)為(a)/(b)=1~3者。若(a)之結構多,則耐熱性提高,但不僅吸水特性變差,而且變脆變硬。因此,使用上述範圍內之多官能化率者。
所使用之環氧樹脂之軟化點(環球法)較佳為50~150℃,進而較佳為52~100℃,尤佳為52~95℃。若為50℃以下,則有黏膩性強烈,操作困難而於生產性方面產生問題之情形。又,於150℃以上之情形時,存在為接近成型溫度之溫度,而無法確保成型時的流動性之情形,故而欠佳。
所使用之環氧樹脂之環氧當量較佳為180~350g/eq.。尤佳為190~300g/eq.。於環氧當量低於180g/eq.之情形時,有官能基過多,因此硬化後之硬化物的吸水率變高,又容易變脆之情形。於環氧當量超過350g/eq.之情形時,認為軟化點變得非常大,或者環氧化未澈底進行,而有氯量變得非常多之情形,故而欠佳。
再者,於本發明中所使用之環氧樹脂之氯量以總氯(水解法)計較佳為200~1500ppm,尤佳成為200~900ppm。根據JPCA之標準,期望即便為環氧單體,氯量亦不超過900ppm。進而,若氯量多,則有多餘氯量影響電氣可靠性之情形,故而欠佳。於氯量低於200ppm之情形時,有需要過度之純化步驟,而於生產性方面產生問題之情形,故而欠佳。
再者,本發明中所使用之環氧樹脂於150℃之熔融黏度較佳為0.05~5Pa.s,尤佳為0.05~2.0Pa.s。若熔融黏度高於5Pa.s,則有流動性產生問題,而加壓時之流暢性或嵌入性產生問題之情形。於熔融黏度低於0.05Pa.s之情形時,有分子量過小,因此耐熱性不足之情形。
上述式中(a)與(b)之比率為(a)/(b)=1~3。即,特徵在於一半以上為間苯二酚結構之環氧丙醚體。本比率對結晶之析出及耐熱性之提高重要,較佳(a)/(b)超過1。又,藉由(a)/(b)為3
以下,而限制間苯二酚結構之環氧丙醚體之量,藉此可改善吸水率與強韌性。
上述式中,n為重複單位,為0~5。藉由n不超過5而控制製成預浸體或樹脂片時之流暢性或流動性。於n超過5之情形時,不僅流動性產生問題,而且於溶劑中之溶解性亦產生問題。
本發明中所使用之環氧樹脂於溶劑中之溶解性變得重要。例如,於併用具有相同骨架之聯苯芳烷基型的環氧樹脂之情形時,關於該等樹脂,亦需要於甲基乙基酮或甲苯、丙二醇單甲醚等溶劑中之溶解性。
於本發明中,尤其於甲基乙基酮中之溶解性係為重要,且要求於5℃、室溫等2個月以上不會析出結晶。與上述(a)/(b)之比率亦有關,若(a)值大,則結晶變得容易析出,因此重要的是(a)/(b)為1以上。
本發明之環氧樹脂組成物係以胺系硬化劑為必須成分。作為可使用之胺系硬化劑,可列舉:二胺基二苯基甲烷、二乙三胺、三乙四胺、二胺基二苯基碸、異佛酮二胺、萘二胺、藉由苯胺與取代聯苯類(4,4'-雙(氯甲基)-1,1'-聯苯及4,4'-雙(甲氧基甲基)-1,1'-聯苯等)、或者取代苯基類(1,4-雙(氯甲基)苯、1,4-雙(甲氧基甲基)苯及1,4-雙(羥甲基)苯等)等之聚縮而獲得之苯胺樹脂等,但並不限定於該等。
尤佳之胺系硬化劑係二官能以上之胺化合物,較佳為下述式所示之結構的樹脂。
(式中,n為重複數,為1~10)。
本發明所使用之胺系硬化劑分別呈現結晶或者樹脂之形狀。
於結晶之情形時,其熔點較佳為35~200℃,尤佳為40~185℃。於熔點之情形時,與軟化點不同,與於其他樹脂中之溶解性亦相關,因此不必如樹脂般一定為成型溫度以下之溫度。
於樹脂之情形時,較佳為50℃~150℃之軟化點(環球法),尤佳為50~100℃。於樹脂之情形時,軟化點為50℃以下者有黏膩性出現問題之情形,故而欠佳,於軟化點超過150℃之情形時,有產生成型時流動性出現問題而無法完全成型,又溶劑無法去除乾淨等問題之情形。
胺化合物之官能基當量較佳為60~600g/eq.(利用電位差滴定之測量)。於活性氫當量為60以下之情形時,有其硬化物於吸水率或強韌性方面產生問題之情形。若活性氫當量超過600,則有耐熱性之維持變得困難之情形。
於本發明之環氧樹脂組成物中,關於胺系硬化劑之使用量,
相對於環氧樹脂之環氧基1當量,以胺化合物之胺當量計,較佳為0.2~0.6當量。尤佳為0.3~0.55當量。於相對於環氧基1當量而未滿0.2當量之情形時,又,超過0.6當量之情形時,有硬化不完全而無法獲得良好之硬化物性之虞,故而欠佳。
本發明之環氧樹脂組成物中亦可含有硬化促進劑。作為可使用之硬化促進劑之具體例,可列舉:甲酸、乙酸、乳酸、乙醇酸、正丁酸、異丁酸、丙酸、己酸、辛酸、正庚酸、單氯乙酸、二氯乙酸、三氯乙酸、硫代乙醇酸、苯酚、間甲酚、對氯酚、對硝基苯酚、2,4-二硝基苯酚、鄰胺基苯酚、對胺基苯酚、2,4,5-三氯苯酚、間苯二酚、對苯二酚、鄰苯二酚、間苯三酚、苯甲酸、對甲苯甲酸、對胺基苯甲酸、對氯苯甲酸、2,4-二氯苯甲酸、水楊酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、蘋果酸、草酸、琥珀酸、丙二酸、富馬酸、馬來酸、酒石酸、檸檬酸等酸;單乙醇胺、二乙醇胺、三乙醇胺等胺類;苯硫酚、2-巰基乙醇、含硫類;2-甲基咪唑、2-乙基咪唑、2-乙基-4-甲基咪唑等咪唑類;2-(二甲胺基甲基)苯酚、1,8-二氮雜雙環[5,4,0]十一碳烯-7等三級胺類;三苯基膦等膦類;辛酸亞錫等金屬化合物等。關於硬化促進劑,相對於環氧樹脂100重量份,可視需要使用0.1~5.0重量份。
本發明之環氧樹脂組成物中,可併用其他環氧樹脂而使用。作為可與式(1)之環氧樹脂併用的其他環氧樹脂之具體例,可列舉:雙酚類(雙酚A、雙酚F、雙酚S、聯苯酚、雙酚AD等)或酚類(苯酚、烷基取代苯酚、芳香族取代苯酚、萘酚、烷基取代萘酚、二羥基苯、烷基取代二羥基苯、二羥基萘等)與各種醛(甲醛、乙醛、烷基醛、苯甲醛、烷基
取代苯甲醛、羥基苯甲醛、萘甲醛、戊二醛、鄰苯二甲醛、巴豆醛、桂皮醛等)之聚縮物;上述酚類與各種二烯化合物(二環戊二烯、萜烯類、乙烯基環己烯、降莰二烯、乙烯基降莰烯、四氫茚、二乙烯基苯、二乙烯基聯苯、二異丙烯基聯苯、丁二烯、異戊二烯等)之聚合物;上述酚類與酮類(丙酮、甲基乙基酮、甲基異丁基酮、苯乙酮、二苯甲酮等)之聚縮物;上述酚類與芳香族二甲醇類(苯二甲醇、聯苯二甲醇等)之聚縮物;上述酚類與芳香族二氯甲基類(α,α'-二氯二甲苯、雙氯甲基聯苯等)之聚縮物;上述酚類與芳香族雙烷氧基甲基類(雙甲氧基甲基苯、雙甲氧基甲基聯苯、雙苯氧基甲基聯苯等)之聚縮物;使上述雙酚類與各種醛之聚縮物或醇類等進行環氧丙基化而成之環氧丙醚系環氧樹脂、脂環式環氧樹脂、環氧丙胺系環氧樹脂、環氧丙酯系環氧樹脂等,只要為通常使用之環氧樹脂則並不限定於該等。該等可單獨使用,亦可使用2種以上。
於摻合本發明之環氧樹脂組成物之情形時,可併用先前公知之硬化劑而使用。作為其他可併用之硬化劑,例如可列舉:酸酐系化合物、醯胺系化合物、酚系化合物、羧酸系化合物等。作為可使用之硬化劑之具體例,可列舉:由二氰二胺、次亞麻油酸之二聚物與乙二胺所合成之聚醯胺樹脂等醯胺系化合物;鄰苯二甲酸酐、苯偏三甲酸酐、均苯四甲酸二酐、馬來酸酐、四氫鄰苯二甲酸酐、甲基四氫鄰苯二甲酸酐、甲基耐地酸酐、六氫鄰苯二甲酸酐、甲基六氫鄰苯二甲酸酐等酸酐系化合物;雙酚A、雙酚F、雙酚S、茀雙酚、萜二酚、4,4'-聯苯酚、2,2'-聯苯酚、3,3',5,5'-四甲基-[1,1'-聯苯]-4,4'-二醇、對苯二酚、間苯二酚、萘二酚、三(4-羥基苯基)甲烷、1,1,2,2-四(4-羥基苯基)乙烷或酚類(苯酚、烷基取代苯酚、
萘酚、烷基取代萘酚、二羥基苯、二羥基萘等)與甲醛、乙醛、苯甲醛、對羥基苯甲醛、鄰羥基苯甲醛、對羥基苯乙酮、鄰羥基苯乙酮、糠醛之聚縮物即酚醛清漆樹脂,或苯酚或甲酚與伸苯基二羥甲基體、二甲氧基甲基體或鹵化甲基體之反應物,或苯酚或甲酚與雙氯甲基聯苯、雙甲氧基甲基聯苯或雙羥甲基聯苯之反應物,或苯酚與苯二異丙醇、苯二異丙醇二甲醚或苯雙(氯異丙烷)之反應物即苯酚芳烷基樹脂及該等之改質物,或四溴雙酚A等鹵化雙酚類,或萜烯與酚類之聚縮物等酚系化合物;咪唑、三氟化硼-胺錯合物、胍衍生物等,但並不限定於該等。該等可單獨使用,亦可使用2種以上。
本發明之環氧樹脂組成物中,亦可含有含磷化合物作為賦予難燃性之成分。作為含磷化合物,可為反應型者亦可為添加型者。作為含磷化合物之具體例,可列舉:磷酸三甲酯、磷酸三乙酯、磷酸三甲酚酯、磷酸三(二甲苯基)酯、磷酸甲酚酯二苯酯、磷酸甲酚酯2,6-二(二甲苯基)酯、1,3-伸苯基雙(磷酸二(二甲苯基)酯)、1,4-伸苯基雙(磷酸二(二甲苯基)酯)、4,4'-聯苯(磷酸二(二甲苯基)酯)等磷酸酯系化合物;9,10-二氫-9-氧雜-10-磷雜菲-10-氧化物、10-(2,5-二羥基苯基)-10H-9-氧雜-10-磷雜菲-10-氧化物等膦類;使環氧樹脂與上述膦類之活性氫進行反應而獲得之含磷環氧化合物、紅磷等,較佳為磷酸酯類、膦類或含磷環氧化合物,尤佳為1,3-伸苯基雙(磷酸二(二甲苯基)酯)、1,4-伸苯基雙(磷酸二(二甲苯基)酯)、4,4'-聯苯(磷酸二(二甲苯基)酯)或含磷環氧化合物。
然而,基於環境問題及電特性之擔憂,如上所述之磷酸酯系化合物之使用量較佳為磷酸酯系化合物/環氧樹脂≦0.1(重量比)。進而較佳為0.05
以下。尤佳除作為硬化促進劑而添加以外,宜不添加磷系化合物。
本發明之環氧樹脂組成物亦可含有無機填充劑。作為無機填充劑,可列舉:熔融二氧化矽、晶質二氧化矽、氧化鋁、碳酸鈣、矽酸鈣、硫酸鋇、滑石、黏土、氧化鎂、氧化鋁、氧化鈹、氧化鐵、氧化鈦、氮化鋁、氮化矽、氮化硼、雲母、玻璃、石英、雲母等。為了進而賦予難燃效果,亦較佳使用氫氧化鎂、氫氧化鋁等金屬氫氧化物。但並不限定於該等。又,亦可混合2種以上而使用。該等無機填充劑中,熔融二氧化矽或晶質二氧化矽等二氧化矽類成本低廉且電可靠性亦良好,故而較佳。
本發明之環氧樹脂組成物中,無機填充劑之使用量以內比例計,通常為5重量%~70重量%、較佳為10重量%~60重量%、更佳為15重量%~60重量%之範圍。若無機填充劑之使用量過少,則有線膨脹變高而翹曲成為問題,或者隨著基板向薄型化方向發展,未出現剛性而於衝程中產生問題之虞。又,若無機填充劑之使用量過多,則有因填料之沈澱等而喪失均質性,或者基板之嵌入性變差,又,與金屬之密接性變差等問題出現之虞,因此於成型為基板時,於剝離或破壞電壓等電特性方面產生不良影響之可能性高。
又,無機填充劑之形狀、粒徑等亦無特別限定,通常為粒徑為0.01~50μm、較佳為0.1~15μm者。
本發明之環氧樹脂組成物中,為了使成型時與模具之脫模變得良好,可摻合脫模劑。作為脫模劑,可使用先前公知者中之任一種,例如可列舉:巴西棕櫚蠟、褐煤蠟等酯系蠟,硬脂酸、棕櫚酸等脂肪酸及該等之金屬鹽,氧化聚乙烯、非氧化聚乙烯等聚烯烴系蠟等。該等可單獨使
用,亦可併用2種以上。該等脫模劑之摻合量相對於全部有機成分,較佳為0.5~3重量%。若過度少於上述範圍,則有自模具之脫模變差之虞,若過度多於上述範圍,則有與基材等之接著變差之虞。
本發明之環氧樹脂組成物中,為了提高無機填充劑與樹脂成分之接著性,可摻合偶合劑。作為偶合劑,可使用先前公知者中之任一種,例如可列舉:乙烯基烷氧基矽烷、環氧烷氧基矽烷、苯乙烯基烷氧基矽烷、甲基丙烯醯氧基烷氧基矽烷、丙烯醯氧基烷氧基矽烷、胺基烷氧基矽烷、巰基烷氧基矽烷、異氰酸酯基烷氧基矽烷等各種烷氧基矽烷化合物,烷氧基鈦化合物、鋁螯合物類等。該等可單獨使用,亦可併用2種以上。關於偶合劑之添加方法,可預先利用偶合劑對無機填充劑表面進行處理後,與樹脂進行混練,亦可於樹脂中混合偶合劑後,混練無機填充劑。
可向本發明之環氧樹脂組成物添加有機溶劑而製成清漆狀之組成物(以下,簡稱為清漆)。作為所使用之溶劑,例如可列舉:γ-丁內酯類、N-甲基吡咯啶酮、N,N-二甲基甲醯胺、N,N-二甲基乙醯胺、N,N-二甲基咪唑啶酮等醯胺系溶劑;四亞甲基碸等碸類;二乙二醇二甲醚、二乙二醇二乙醚、丙二醇、丙二醇單甲醚、丙二醇單甲醚單乙酸酯、丙二醇單丁醚等醚系溶劑;甲基乙基酮、甲基異丁基酮、環戊酮、環己酮等酮系溶劑;甲苯、二甲苯等芳香族系溶劑。溶劑係於所獲得之清漆中之除溶劑以外的固形分濃度成為通常10~80重量%、較佳為20~70重量%之範圍內使用。
進而,可視需要向本發明之環氧樹脂組成物中摻合公知之添加劑。作為可使用之添加劑之具體例,可列舉:聚丁二烯及其改質物、丙
烯腈共聚物之改質物、聚苯醚、聚苯乙烯、聚乙烯、聚醯亞胺、氟樹脂、馬來醯亞胺系化合物、氰酸酯系化合物、聚矽氧凝膠、聚矽氧油、以及碳黑、酞菁藍、酞菁綠等著色劑等。
對本發明之樹脂片進行說明。
使用本發明之環氧樹脂組成物之樹脂片係藉由本身公知之凹版塗佈法、網版印刷、金屬掩模法、旋轉塗佈法等各種塗佈方法,將上述清漆以乾燥後之厚度成為特定厚度、例如5~100μm之方式塗佈於平面狀支持體上之後,進行乾燥而獲得,但使用何種塗佈方法係根據支持體之種類、形狀、尺寸、塗佈之膜厚、支持體之耐熱性等而適當選擇。
作為平面支持體,例如可列舉:由聚醯胺、聚醯胺醯亞胺、聚芳酯、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚醚酮、聚醚醯亞胺、聚醚醚酮、聚酮、聚乙烯、聚丙烯、鐵氟龍(註冊商標)等各種高分子、及/或其共聚物所製作之膜、或者銅箔等金屬箔等。
塗佈後進行乾燥,可獲得片狀之組成物(本發明之樹脂片),但亦可藉由將本樹脂片進一步進行加熱而製成片狀之硬化物。又,亦可以一次加熱兼任溶劑乾燥與硬化步驟。
關於本發明之環氧樹脂組成物,可藉由上述方法對上述支持體之兩面或單面進行塗佈,並加熱,藉此於該支持體之兩面或單面形成硬化物之層。又,亦可藉由在硬化前貼合被接著體,使之硬化而製作積層體。
又,本發明之樹脂片亦可藉由自支持體剝離而用作接著片,亦可與被接著體進行接觸,視需要施加壓力與熱,而使硬化與接著一併進行。
對本發明之預浸體進行說明。
本發明之預浸體係使上述本發明之環氧樹脂組成物含浸於纖維基材而成者。藉此,可獲得耐熱性、低膨脹性及難燃性優異之預浸體。作為上述纖維基材,例如可列舉:玻璃織布、玻璃不織布、玻璃紙等玻璃纖維基材;由紙、聚芳醯胺、聚酯、芳香族聚酯、氟樹脂等合成纖維等構成之織布或不織布;由金屬纖維、碳纖維、礦物纖維等構成之織布、不織布、墊子(mat)類等。該等基材可單獨使用或者亦可混合使用。該等中,較佳為玻璃纖維基材。藉此,可進一步提高預浸體之剛性、尺寸穩定性。
作為玻璃纖維基材,較佳含有選自由T玻璃、S玻璃、E玻璃、NE玻璃、及石英玻璃組成之群中之至少一種者。
關於使本發明之環氧樹脂組成物含浸於上述纖維基材之方法,例如可列舉:將基材浸漬於樹脂清漆中之方法、利用各種塗佈機進行塗佈之方法、利用噴霧器進行吹附之方法等。該等中,較佳將基材浸漬於樹脂清漆中之方法。藉此,可提高樹脂組成物對基材之含浸性。再者,於將基材浸漬於樹脂清漆中之情形時,可使用通常之含浸塗佈設備。
例如,使本發明之環氧樹脂組成物直接,或者以溶解或分散於溶劑中而成之清漆的形態含浸於玻璃布等基材之後,於乾燥爐中等,於通常80~200℃(其中,於使用溶劑之情形時,設為可使溶劑揮發之溫度以上)下乾燥2~30分鐘、較佳為2~15分鐘,藉此獲得預浸體。
對本發明之覆金屬積層板進行說明。
本發明中所使用之積層板係將上述本發明之預浸體進行加熱加壓成形而成者。藉此,可獲得耐熱性、低膨脹性及難燃性優異之覆金屬積層板。於為1片預浸體時,於其上下兩面或單面重疊金屬箔。又,亦可將2片以
上之預浸體進行積層。於將2片以上之預浸體進行積層時,於積層之預浸體的最外側之上下兩面或單面重疊金屬箔或膜。其次,對將預浸體與金屬箔重疊而成者進行加熱加壓成形,藉此可獲得覆金屬積層板。上述進行加熱之溫度並無特別限定,較佳為120~220℃,尤佳為150~200℃。上述進行加壓之壓力並無特別限定,較佳為1.5~5MPa,尤佳為2~4MPa。又,視需要亦可於高溫槽等中於150~300℃之溫度下進行後硬化。
對本發明之印刷配線基板進行說明。
本發明之印刷配線基板係使用上述本發明之覆金屬積層板作為內層電路基板。於覆金屬積層板之單面或兩面進行電路形成。視情形亦可藉由鑽孔加工、雷射加工而形成通孔,並藉由鍍敷等而實現兩面之電連接。
可於上述內層電路基板上重疊市售或本發明之樹脂片,或者上述本發明之預浸體並進行加熱加壓成形,而獲得多層印刷配線基板。
具體而言,可藉由將上述樹脂片之絕緣層側與內層電路基板進行重疊,使用真空加壓式貼合裝置等進行真空加熱加壓成形,其後,利用熱風乾燥裝置等使絕緣層加熱硬化而獲得。
此處,作為進行加熱加壓成形之條件,並無特別限定,若舉一例,則可於溫度60~160℃,壓力0.2~3MPa實施。又,作為進行加熱硬化之條件,並無特別限定,若舉一例,則可於溫度140~240℃實施30~120分鐘。
或者,亦可藉由使上述本發明之預浸體重疊於內層電路基板,使用平板加壓裝置等對其進行加熱加壓成形而獲得。此處,作為進行加熱加壓成形之條件,並無特別限定,若舉一例,則可於溫度140~240℃,壓力1~4MPa實施。於此種利用平板加壓裝置等所進行之加熱加壓成形中,於加熱加壓
成形之同時進行絕緣層之加熱硬化。
又,本發明之多層印刷配線基板之製造方法包括:將上述樹脂片或本發明之預浸體,重疊於內層電路基板之形成有內層電路圖案之面並進行連續積層的步驟,及藉由半加成法而形成導體電路層之步驟。
關於由上述樹脂片或本發明之預浸體形成之絕緣層之硬化,亦有為了使接下來之雷射照射及樹脂殘渣之去除變得容易,提高除膠渣(desmear)性,而預先設為半硬化狀態之情形。又,將第一層之絕緣層在低於通常之加熱溫度之溫度進行加熱,藉此使一部分硬化(半硬化),於絕緣層上,進而形成一層乃至複數層絕緣層,使半硬化之絕緣層再次加熱硬化至實用上無問題之程度,藉此可使絕緣層間及絕緣層與電路間之密接力提高。該情形時之半硬化之溫度較佳為80℃~200℃,更佳為100℃~180℃。再者,於後續步驟中,照射雷射而於絕緣層形成開口部,但在此之前必須將基材進行剝離。關於基材之剝離,即便於形成絕緣層後、加熱硬化之前、或加熱硬化後中之任一時間點進行,亦無特別問題。
再者,獲得上述多層印刷配線基板時所使用之內層電路基板例如可適宜地使用藉由蝕刻等而於覆銅積層板之兩面形成特定之導體電路,對導體電路部分進行黑化處理而成者。
雷射照射後之樹脂殘渣等較佳利用過錳酸鹽、重鉻酸鹽等氧化劑等而去除。又,可同時使平滑之絕緣層之表面粗化,而可提高後續藉由金屬鍍敷所形成之導電配線電路的密接性。
其次,形成外層電路。外層電路之形成方法係藉由金屬鍍敷而實現絕緣樹脂層間之連接,並藉由蝕刻而進行外層電路圖案形成。可與
使用樹脂片或預浸體時同樣地進行,而獲得多層印刷配線基板。
再者,於使用具有金屬箔之樹脂片或預浸體之情形時,為了不剝離金屬箔而用作導體電路,藉由蝕刻進行電路形成。於該情形時,若利用使用厚銅箔之附帶基材的絕緣樹脂片,則於其後之電路圖案形成中微間距化變得困難,因此亦有使用1~5μm之極薄銅箔,或者進行藉由蝕刻而使12~18μm之銅箔變薄至1~5μm之半蝕刻的情形。
亦可進而積層絕緣層,並進行與上述相同之電路形成,但對於多層印刷配線基板之設計而言,於最外層進行電路形成後,形成阻焊(solder resist)層。阻焊層之形成方法並無特別限定,例如藉由如下方法而形成:藉由將乾膜型之阻焊層進行積層(層壓),並進行曝光及顯影而形成之方法;或者藉由對印刷有液狀抗蝕劑者進行曝光及顯影而形成之方法。再者,於將所獲得之多層印刷配線基板用於半導體裝置之情形時,為了安裝半導體元件而設置連接用電極部。連接用電極部可由鍍金、鍍鎳及焊料鍍敷等之金屬皮膜適當被覆。藉由上述方法可製造多層印刷配線基板。
其次,對本發明之半導體裝置進行說明。
於上述中所獲得之多層印刷配線基板上安裝具有焊接凸塊之半導體元件,而實現經由焊接凸塊而與上述多層印刷配線基板之連接。然後,於多層印刷配線基板與半導體元件之間填充液狀密封樹脂而形成半導體裝置。焊接凸塊較佳由合金構成,該合金係由錫、鉛、銀、銅、鉍等構成。
關於半導體元件與多層印刷配線基板之連接方法,係使用倒裝晶片接合機等進行基板上之連接用電極部與半導體元件的焊接凸塊之位置對準後,使用IR回流焊(IR reflow)裝置、熱板、其他加熱裝置將焊接凸塊加熱至
熔點以上,將多層印刷配線基板與焊接凸塊進行熔融接合,藉此進行連接。再者,為了使連接可靠性變良好,亦可預先於多層印刷配線基板上之連接用電極部形成焊膏等熔點相對較低之金屬層。亦可於該接合步驟之前,於焊接凸塊及、或多層印刷配線基板上之連接用電極部之表層塗佈助焊劑,藉此提高連接可靠性。
作為基板,係用於母板、網狀基板、封裝基板等,並作為基板使用。尤其是作為封裝基板,作為單面密封材料用之薄層基板而有用。又,於用作半導體密封材之情形時,作為根據其摻合獲得之半導體裝置,例如可列舉:DIP(Dual inline package,雙列直插封裝)、QFP(Quad Flat Package,四面扁平封裝)、BGA(Ball Grid Array,球狀柵格陣列)、CSP(Chip Scale Package,晶片尺寸封裝)、SOP(Small Outline Package,小尺寸封裝)、TSOP(Thin Small Outline Package,薄型小尺寸封裝)、TQFP(Thin Quad Flat Package,薄型四方扁平封裝)等。
實施例
以下列舉合成例及實施例,對本發明之特徵進一步具體地進行說明。關於以下所示之材料、處理內容、處理順序等,只要不偏離本發明之主旨則可適當變更。因此,本發明之範圍並非應受以下所示之具體例限定性地加以解釋者。
此處,各物性值之測量條件係如下所述。
.環氧當量
藉由JIS K-7236所記載之方法進行測量,單位為g/eq.。
.軟化點
藉由依據JIS K-7234之方法進行測量,單位為℃。
.彈性模數(DMA)
動態黏彈性測量器:TA-instruments,DMA-2980
測量溫度範圍:-30~280℃
升溫速度:2℃/min
試片尺寸:使用切割為5mm×50mm者
Tg:將DMA測量中Tan-δ之波峰點設為Tg
.吸水率
將直徑5cm×厚度4mm之圓盤狀試片於100℃之水中煮沸72小時後的重量增加率(%)
合成例1
於具備攪拌機、回流冷卻管、攪拌裝置之燒瓶中,一面實施氮氣沖洗,一面添加依據WO2007/007827而製造之下述式所示之酚樹脂((a)/(b)=1.3n=1.5羥基當量134g/eq.軟化點93℃)134份、表氯醇450份、甲醇54份,於攪拌下進行溶解,並升溫至70℃。繼而,耗費90分鐘分批添加薄片狀之氫氧化鈉42.5份後,進而於70℃反應1小時。反應結束後,進行水洗,將鹽去除後,針對所獲得之有機層,使用旋轉蒸發器,於減壓下將過量之表氯醇等溶劑類蒸餾去除。對殘留物添加甲基異丁基酮500份並進行溶解,於攪拌下添加30重量%之氫氧化納水溶液17份,進行1小時反應後,進行水洗直至油層之清洗水成為中性,使用旋轉蒸發器,於減壓下自所獲得之溶液蒸餾去除甲基異丁基酮等,藉此獲得式(1)之環氧樹脂(EP1)195份。所獲得之環氧樹脂之環氧當量為211g/eq.,軟化點為71℃,
150℃之熔融黏度(ICI熔融黏度 圓錐#1)為0.34Pa.s。
實施例1
針對合成例1中所獲得之環氧樹脂(EP1),相對於環氧當量1莫耳當量而摻合A-1(胺當量198g/eq,活性氫當量97.5g/eq,軟化點55℃)0.5當量作為硬化劑,以相對於環氧樹脂100重量份成為1重量份之比例(重量份)摻合水楊酸作為觸媒,並使用混合輥均勻地混合、混練而獲得環氧樹脂組成物。利用攪拌器粉碎該環氧樹脂組成物,進而利用壓錠機進行錠化。將該經錠化之環氧樹脂組成物進行轉注成型(175℃×60秒),進而脫模後於160℃×2小時+180℃×6小時之條件下進行硬化,而獲得評價用試片。將評價結果示於表1。
再者,評價所使用之環氧樹脂的詳細情況示於以下之表2。
比較例1~7
實施例1中,針對合成例1中所獲得之環氧樹脂(EP1)、及各種環氧樹脂,使用等當量之A-1或HA-1(明和化成工業(股份)製造之酚系酚醛清漆樹脂)作為硬化劑,且使用三苯基膦(TPP)或水楊酸作為觸媒,藉由與實施例1相同之調配、方法獲得比較用之評價用試片。將評價結果示於表1。
根據表1確認,若將實施例1與比較例3進行比較,則與使用酚樹脂作為硬化劑之情況相比,藉由使用胺系硬化劑可特異性地形成耐熱性及吸水特性良好之硬化物。
又,將針對表1中所獲得之硬化物性,以耐熱性(Tg)為橫軸,以吸水特性(%)為縱軸所繪製之圖表示於圖1。
由圖1確認,比較例1~3、比較例4~7之硬化物具有若Tg上升則吸水率上升之相關關係。相對於此,可確認使用式(1)之環氧樹脂與胺系硬化劑之硬化物儘管具有高耐熱性,但吸水率低,係與上述相關關係不同之特異性組合。
參照特定態樣對本發明詳細地進行了說明,但從業者明瞭可在不偏離本發明之精神與範圍之情況下進行各種變更及修正。
再者,本申請案係基於2014年8月1日提出申請之日本專利申請案(日本特願2014-157629),藉由引用而援用其全文。又,此處所引用之全部參照係將全文併入本文中。
[產業上之可利用性]
本發明之環氧樹脂組成物提供其硬化物,該硬化物可同時達成高耐熱性與耐水性,因此係對製作印刷配線基板或增層基板等積層板極有用之材料。
Claims (9)
- 一種環氧樹脂組成物,其以下述通式(1)所示之環氧樹脂與胺系硬化劑為必須成分,
- 一種預浸體,其係使申請專利範圍第1項之環氧樹脂組成物含浸於纖維基材而成。
- 如申請專利範圍第2項之預浸體,其中該纖維基材為玻璃纖維基材。
- 如申請專利範圍第3項之預浸體,其中該玻璃纖維基材含有選自由T玻璃、S玻璃、E玻璃、NE玻璃、及石英玻璃組成之群中之至少1種。
- 一種覆金屬積層板,其於申請專利範圍第2至4項中任一項之預浸體之至少一面積層有金屬箔。
- 一種樹脂片,其係將由申請專利範圍第1項之環氧樹脂組成物構成之絕緣層形成於膜上或金屬箔上而成。
- 一種印刷配線基板,其係將申請專利範圍第5項之覆金屬積層板用於內層電路基板而成。
- 一種印刷配線基板,其係使申請專利範圍第2至4項中任一項之預浸體或申請專利範圍第6項之樹脂片進行硬化而成。
- 一種半導體裝置,其係於申請專利範圍第7或8項之印刷配線基板搭 載半導體元件而成。
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KR (1) | KR102316144B1 (zh) |
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TWI672336B (zh) * | 2017-03-22 | 2019-09-21 | 南韓商Lg化學股份有限公司 | 用於半導體封裝的樹脂組成物以及使用此組成物的預浸料以及金屬包覆層壓板 |
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WO2018174447A1 (ko) * | 2017-03-22 | 2018-09-27 | 주식회사 엘지화학 | 반도체 패키지용 수지 조성물과 이를 이용한 프리프레그 및 금속박 적층판 |
KR102057255B1 (ko) * | 2017-03-22 | 2019-12-18 | 주식회사 엘지화학 | 반도체 패키지용 수지 조성물과 이를 이용한 프리프레그 및 금속박 적층판 |
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KR102246974B1 (ko) * | 2018-04-10 | 2021-04-30 | 주식회사 엘지화학 | 반도체 패키지용 열경화성 수지 조성물, 프리프레그 및 금속박 적층판 |
KR102257926B1 (ko) * | 2018-09-20 | 2021-05-28 | 주식회사 엘지화학 | 다층인쇄회로기판, 이의 제조방법 및 이를 이용한 반도체 장치 |
JP6636599B2 (ja) * | 2018-11-30 | 2020-01-29 | 日本化薬株式会社 | エポキシ樹脂組成物、プリプレグ及び金属張積層板、プリント配線基板 |
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JPH05170874A (ja) * | 1991-12-19 | 1993-07-09 | Mitsui Toatsu Chem Inc | エポキシ樹脂組成物 |
JP3476027B2 (ja) * | 1994-04-28 | 2003-12-10 | 日本化薬株式会社 | エポキシ樹脂の製造方法 |
JP3525152B2 (ja) * | 1996-09-30 | 2004-05-10 | 独立行政法人 科学技術振興機構 | エポキシ樹脂硬化性組成物 |
JP2004189811A (ja) * | 2002-12-10 | 2004-07-08 | Toho Tenax Co Ltd | 織物プリプレグ |
JP5195582B2 (ja) * | 2009-03-30 | 2013-05-08 | 日立化成株式会社 | 熱硬化性絶縁樹脂組成物、並びにこれを用いた支持体付絶縁フィルム、プリプレグ、積層板及び多層プリント配線板 |
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JP5754731B2 (ja) * | 2011-08-25 | 2015-07-29 | 明和化成株式会社 | エポキシ樹脂、エポキシ樹脂の製造方法、及びその使用 |
KR101295688B1 (ko) | 2011-10-21 | 2013-08-14 | 부산대학교 산학협력단 | 유체의 회전을 이용한 액화천연가스 저장탱크의 슬로싱 저감장치 |
JP6410405B2 (ja) * | 2012-08-01 | 2018-10-24 | 住友ベークライト株式会社 | 樹脂基板、プリプレグ、プリント配線基板、半導体装置 |
CN103897143B (zh) * | 2012-12-28 | 2018-05-01 | 明和化成株式会社 | 环氧树脂、环氧树脂的制造方法及其使用 |
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WO2016017751A1 (ja) | 2016-02-04 |
CN106661200B (zh) | 2019-12-24 |
JP2016034996A (ja) | 2016-03-17 |
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