TWI728066B - 樹脂薄片 - Google Patents
樹脂薄片 Download PDFInfo
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- TWI728066B TWI728066B TW106107994A TW106107994A TWI728066B TW I728066 B TWI728066 B TW I728066B TW 106107994 A TW106107994 A TW 106107994A TW 106107994 A TW106107994 A TW 106107994A TW I728066 B TWI728066 B TW I728066B
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- Prior art keywords
- resin
- resin composition
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Abstract
提供一種可賦予絕緣性能為優異的薄絕緣層的樹脂薄片。
本發明之樹脂薄片,其係包含支撐體、與接合在該支撐體上的樹脂組成物層,該樹脂組成物層之硬化物在120℃下20小時的萃取水導電率A為50μS/cm以下,且該樹脂組成物層之硬化物在160℃下20小時的萃取水導電率B為200μS/cm以下。
Description
本發明係關於樹脂薄片。進而係關於包含該樹脂薄片之樹脂組成物層之硬化物之印刷配線板、及半導體裝置。
近年為達成電子機器之小型化,進行著印刷配線板之更進一步之薄型化,故內層基板或絕緣層之厚度有變得更薄之傾向。作為減小內層基板或絕緣層之厚度者,已知有例如專利文獻1所記載之薄型薄片用樹脂組成物。
[先前技術文獻]
[專利文獻]
[專利文獻1]日本特開2014-152309號公報
專利文獻1中,本發明人發現將薄膜薄片適
用在絕緣層時,會有粗度變大、剝離強度降低之傾向,為了解決該等的課題而提案將熱可塑性樹脂的調配量設為指定量。然而,該文獻中,對於減小絕緣層之厚度時之絕緣性能(以下亦稱為「薄膜絕緣性」)並無任何研討。
若絕緣層為薄膜之情形時,無機填充材粒子彼此會接觸而透過界面傳遞使得電流變得容易流動、或因為絕緣層之厚度為薄而靜電容量變大導致容易短路等,維持相較以往之絕緣性能將為困難。
本發明之課題係提供一種可賦予絕緣性能為優異的薄絕緣層之樹脂薄片。
為解決上述課題經深入研究之結果,本發明人發現在包含支撐體、與接合在該支撐體上的樹脂組成物層之樹脂薄片中,藉由樹脂組成物層之硬化物為滿足指定的萃取水導電率、及指定的拉伸破壞強度比中之至少一者,即便是厚度薄亦可賦予絕緣性能為優異的(薄膜絕緣性為優異)的絕緣層。詳細而言,本發明人發現:藉由降低硬化物在高溫下之萃取水導電率、或抑制將硬化物配置在高溫高濕度環境下時之拉伸破壞強度之降低,可賦予薄膜絕緣性為優異的絕緣層,進而完成本發明。
即,本發明係包含以下之內容。
[1].一種樹脂薄片,其係包含支撐體、與接合在該支撐體上的樹脂組成物層,該樹脂組成物層之硬化物在120
℃下20小時的萃取水導電率A為50μS/cm以下,且該樹脂組成物層之硬化物在160℃下20小時的萃取水導電率B為200μS/cm以下。
[2].如前述[1]之樹脂薄片,其中,樹脂組成物層之硬化物的玻璃移轉溫度為160℃以上。
[3].一種樹脂薄片,其係包含支撐體、與接合在該支撐體上的樹脂組成物層,該樹脂組成物層之硬化物且厚度為10μm之硬化物之HAST試驗後之拉伸破壞強度B,對該樹脂組成物層之硬化物且厚度為10μm之硬化物之拉伸破壞強度A之比(B/A)為0.65以上1以下。
[4].如前述[3]之樹脂薄片,其中,前述拉伸破壞強度B為50MPa以上。
[5].如前述[1]~[4]中任一項之樹脂薄片,其中,樹脂組成物層之厚度為15μm以下。
[6].如前述[1]~[5]中任一項之樹脂薄片,其中,樹脂組成物層之最低熔融黏度為1000poise以上。
[7].如前述[1]~[6]中任一項之樹脂薄片,其中,樹脂組成物層含有環氧樹脂及硬化劑。
[8].如前述[1]~[7]中任一項之樹脂薄片,其中,若樹脂組成物層含有無機填充材、且將樹脂組成物層中之不揮發成分設為100質量%時,該無機填充材的含有量為50質量%以上。
[9].如前述[8]之樹脂薄片,其中,該無機填充材之平均粒徑為0.05μm~0.35μm。
[10].如前述[8]或[9]之樹脂薄片,其中,該無機填充材之比表面積[m2/g]與真密度[g/cm3]之乘積為0.1~77。
[11].如前述[1]~[10]中任一項之樹脂薄片,其係印刷配線板之絕緣層形成用。
[12].如前述[1]~[11]中任一項之樹脂薄片,其係包含第1導體層、第2導體層、與絕緣第1導體層和第2導體層的絕緣層、且第1導體層和第2導體層之間的絕緣層之厚度為6μm以下的印刷配線板之該絕緣層形成用。
[13].一種印刷配線板,其係包含第1導體層、第2導體層、與絕緣第1導體層和第2導體層的絕緣層、且第1導體層和第2導體層之間的絕緣層之厚度為6μm以下,該絕緣層係前述[1]~[12]中任一項之樹脂薄片之樹脂組成物層之硬化物。
[14].一種半導體裝置,其係包含前述[13]之印刷配線板。
依據本發明可提供一種可賦予絕緣性能為優異的薄絕緣層之樹脂薄片。
5‧‧‧第1導體層
51‧‧‧第1導體層之主面
6‧‧‧第2導體層
61‧‧‧第2導體層之主面
7‧‧‧絕緣層
[圖1]圖1係示意性表示印刷配線板之一例之部分截面圖。
[實施發明之最佳形態]
以下,對於本發明之樹脂薄片、具備有該樹脂薄片之樹脂組成物層之硬化物之印刷配線板、及半導體裝置來進行詳細說明。
本發明之樹脂薄片係包含支撐體、與接合在該支撐體上的樹脂組成物層。本發明中,其特徵為樹脂組成物層之硬化物,如以下表示般滿足特定的萃取水導電率(特性1)及特定的拉伸破壞強度比(特性2)之中至少一者。
尚,對於特性2中言及所謂的「樹脂組成物層之硬化物且厚度為10μm之硬化物之拉伸破壞強度A」,係指「該厚度為10μm之情形時,樹脂組成物層之硬化物呈現之HAST試驗前之拉伸破壞強度A」之意,又所謂的「樹脂組成物層之硬化物且厚度為10μm之硬化物之HAST試驗後之拉伸破壞強度B」,係指「該厚度為10μm之情形時,樹脂組成物層之硬化物呈現之HAST試驗後之拉伸破壞強度B」之意味。特性2並非限定樹脂薄片中之樹脂組成物層之厚度。
(特性1)樹脂組成物層之硬化物在120℃下20小時之萃取水導電率A為50μS/cm以下、且樹脂組成物層之硬化物在160℃下20小時之萃取水導電率B為200μS/cm以下。
(特性2)樹脂組成物層之硬化物且厚度為10μm之硬化物之HAST試驗後之拉伸破壞強度B,對樹脂組成物層
之硬化物且厚度為10μm之硬化物之拉伸破壞強度A之比(B/A)為0.65以上1以下。
樹脂組成物層係藉由樹脂組成物來形成。首先,對於形成樹脂組成物層之樹脂組成物來進行說明。
[樹脂組成物]
樹脂組成物並無特別限定,只要是藉由樹脂組成物所形成之樹脂組成物層之硬化物滿足上述特性1及特性2之中至少一者即可。作為賦予滿足特性1及特性2之中至少一者之硬化物之樹脂組成物,可舉例如包含硬化性樹脂與該硬化劑之組成物。作為硬化性樹脂,可使用在形成印刷配線板之絕緣層之際所使用的以往周知的硬化性樹脂,其中,以環氧樹脂為較佳。因此,一實施形態中,樹脂組成物係含有(A)環氧樹脂及(B)硬化劑。樹脂組成物係以含有(C)無機填充材者為較佳。樹脂組成物進而因應所需亦可包含熱可塑性樹脂、硬化促進劑、耐燃劑及有機填充材等的添加劑。
以下,對於可使用作為樹脂組成物之材料之(A)環氧樹脂、(B)硬化劑、(C)無機填充材及添加劑來進行說明。
<(A)環氧樹脂>
作為(A)環氧樹脂,可舉例如雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、雙酚AF型環氧樹
脂、雙環戊二烯型環氧樹脂、三酚(trisphenol)型環氧樹脂、萘酚酚醛清漆型環氧樹脂、苯酚酚醛清漆型環氧樹脂、tert-丁基-兒茶酚型環氧樹脂、萘型環氧樹脂、萘酚型環氧樹脂、蒽型環氧樹脂、縮水甘油胺型環氧樹脂、縮水甘油酯型環氧樹脂、甲酚酚醛清漆型環氧樹脂、聯苯型環氧樹脂、線狀脂肪族環氧樹脂、具有丁二烯構造之環氧樹脂、脂環式環氧樹脂、雜環式環氧樹脂、含有螺環的環氧樹脂、環己烷二甲醇型環氧樹脂、伸萘基醚型環氧樹脂、三羥甲基型環氧樹脂、四苯乙烷型環氧樹脂等。環氧樹脂係可1種單獨使用,亦可組合2種以上來使用。(A)成分係以選自雙酚A型環氧樹脂、雙酚F型環氧樹脂、及聯苯型環氧樹脂之1種以上為較佳。
環氧樹脂係以包含在1分子中具有2個以上的環氧基之環氧樹脂為較佳。將環氧樹脂的不揮發成分設為100質量%時,至少50質量%以上係以在1分子中具有2個以上的環氧基之環氧樹脂為較佳。其中,以包含在1分子中具有2個以上的環氧基、且在溫度20℃下為液狀的環氧樹脂(以下稱為「液狀環氧樹脂」)、與在1分子中具有3個以上的環氧基、且在溫度20℃下為固體狀的環氧樹脂(以下稱為「固體狀環氧樹脂」)為較佳。作為環氧樹脂,藉由併用液狀環氧樹脂與固體狀環氧樹脂,從而具有優異的可撓性、且硬化物之斷裂強度亦為提升。特別是固體狀環氧樹脂之耐熱性為高,容易使硬化物在高溫下之萃取水導電率降低,且將硬化物設置在高溫高濕度下時可
容易抑制拉伸破壞強度之降低。
作為液狀環氧樹脂,以雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚AF型環氧樹脂、萘型環氧樹脂、縮水甘油酯型環氧樹脂、縮水甘油胺型環氧樹脂、苯酚酚醛清漆型環氧樹脂、具有酯骨架之脂環式環氧樹脂、環己烷二甲醇型環氧樹脂、縮水甘油胺型環氧樹脂、及具有丁二烯構造之環氧樹脂為較佳,以縮水甘油胺型環氧樹脂、雙酚A型環氧樹脂、雙酚F型環氧樹脂、雙酚AF型環氧樹脂及萘型環氧樹脂為又較佳。作為液狀環氧樹脂之具體例,可舉出DIC(股)製的「HP4032」、「HP4032D」、「HP4032SS」(萘型環氧樹脂)、三菱化學(股)製的「828US」、「jER828EL」(雙酚A型環氧樹脂)、「jER807」(雙酚F型環氧樹脂)、「jER152」(苯酚酚醛清漆型環氧樹脂)、「YL7760」(雙酚AF型環氧樹脂)、「630」、「630LSD」(縮水甘油胺型環氧樹脂)、新日鐵住金化學(股)製的「ZX1059」(雙酚A型環氧樹脂與雙酚F型環氧樹脂的混合品)、新日鐵住金化學(股)製「YD-8125G」(雙酚A型環氧樹脂)、Nagasechemtex(股)製的「EX-721」(縮水甘油酯型環氧樹脂)、Daicel(股)製的「CELLOXIDE 2021P」(具有酯骨架之脂環式環氧樹脂)、「PB-3600」(具有丁二烯構造之環氧樹脂)、新日鐵化學(股)製的「ZX1658」、「ZX1658GS」(液狀1,4-縮水甘油環己烷)、三菱化學(股)製的「630LSD」(縮水甘油胺型環氧樹脂)等。該等係可1種單獨使用,亦可組合2
種以上來使用。
作為固體狀環氧樹脂,以萘型4官能環氧樹脂、甲酚酚醛清漆型環氧樹脂、雙環戊二烯型環氧樹脂、三酚型環氧樹脂、萘酚型環氧樹脂、聯苯型環氧樹脂、伸萘基醚型環氧樹脂、蒽型環氧樹脂、雙酚A型環氧樹脂、四苯乙烷型環氧樹脂為較佳,以萘型4官能環氧樹脂、萘酚型環氧樹脂、及聯苯型環氧樹脂為又較佳。作為固體狀環氧樹脂之具體例,可舉出DIC(股)製的「HP4032H」(萘型環氧樹脂)、「HP-4700」、「HP-4710」(萘型4官能環氧樹脂)、「N-690」(甲酚酚醛清漆型環氧樹脂)、「N-695」(甲酚酚醛清漆型環氧樹脂)、「HP-7200」、「HP-7200HH」、「HP-7200H」(雙環戊二烯型環氧樹脂)、「EXA-7311」、「EXA-7311-G3」、「EXA-7311-G4」、「EXA-7311-G4S」、「HP6000」(伸萘基醚型環氧樹脂)、日本化藥(股)製的「EPPN-502H」(三酚型環氧樹脂)、「NC7000L」(萘酚酚醛清漆型環氧樹脂)、「NC3000H」、「NC3000」、「NC3000L」、「NC3100」(聯苯型環氧樹脂)、新日鐵住金化學(股)製的「ESN475V」(萘型環氧樹脂)、「ESN485」(萘酚酚醛清漆型環氧樹脂)、三菱化學(股)製的「YX4000H」、「YL6121」(聯苯型環氧樹脂)、「YX4000HK」(聯二甲酚型環氧樹脂)、「YX8800」(蒽型環氧樹脂)、大阪Gas Chemicals(股)製的「PG-100」、「CG-500」、三菱化學(股)製的「YL7800」(茀型環氧樹脂)、三菱化學(股)製的
「jER1010」、(固體狀雙酚A型環氧樹脂)、「jER1031S」(四苯乙烷型環氧樹脂)等。
就使樹脂組成物層之硬化物之萃取水導電率降低,且將樹脂組成物層之硬化物配置在高溫高濕度環境下時可抑制拉伸破壞強度之降低之觀點而言,作為環氧樹脂,以純度為高的樹脂(例如氯離子等的離子性雜質較少的樹脂等)為較佳。作為純度為高的環氧樹脂,可舉例如三菱化學(股)製的「828US」、「YL980」、「1750」、「YL983U」、新日鐵住金化學(股)製「YD-8125G」、「YD-825GS」、「ZX-1658GS」、「YDF-8170G」等。
作為液狀環氧樹脂,係以在1分子中具有2個以上的環氧基、且在溫度20℃下液狀的芳香族系環氧樹脂為較佳,作為固體狀環氧樹脂,係以在1分子中具有3個以上的環氧基、且在溫度20℃下固體狀的芳香族系環氧樹脂為較佳。尚,本發明中所言及所謂的芳香族系環氧樹脂,係指在該分子內具有芳香環構造之環氧樹脂之意。
作為環氧樹脂,併用液狀環氧樹脂與固體狀環氧樹脂之情形時,此等之量比(液狀環氧樹脂:固體狀環氧樹脂)係就質量比計,以1:1.0~1:15的範圍內為較佳。藉由將液狀環氧樹脂與固體狀環氧樹脂的量比設為上述範圍內可得到:i)以樹脂薄片之形態來使用之情形時能產生適度的黏著性、ii)以樹脂薄片之形態來使用之情形時,可得到充分的可撓性、且操作性提升、以及iii)具有充分的斷裂強度之樹脂組成物層之硬化物等的效果。就上述i)~iii)
的效果之觀點而言,液狀環氧樹脂與固體狀環氧樹脂的量比(液狀環氧樹脂:固體狀環氧樹脂)係就質量比計,以1:2.0~1:12的範圍內為又較佳,1:3.0~1:10的範圍內為更佳。
樹脂組成物中之環氧樹脂的含有量,就可得到展現出良好的拉伸破壞強度、絕緣可靠性之絕緣層之觀點而言,較佳為5質量%以上,又較佳為9質量%以上,更佳為13質量%以上。環氧樹脂的含有量之上限,只要可發揮本發明之效果即可,並無特別限定,較佳為50質量%以下,又較佳為40質量%以下。
尚,本發明中,樹脂組成物中之各成分的含有量,只要是無另外特別說明時,為將樹脂組成物中之不揮發成分設成100質量%時的值。
環氧樹脂的環氧當量,較佳為50~5000,又較佳為50~3000,更佳為80~2000,更又較佳為110~1000。藉由成為此範圍內,從而可產生樹脂組成物層之硬化物之交聯密度成為充分且表面粗度為小的絕緣層。尚,環氧當量係可根據JIS K7236來進行測定,為包含1當量的環氧基之樹脂的質量。
環氧樹脂的重量平均分子量係較佳為100~5000,又較佳為250~3000,更佳為400~1500。於此,環氧樹脂的重量平均分子量係藉由凝膠滲透層析法(GPC)法所測定之聚苯乙烯換算的重量平均分子量。
<(B)硬化劑>
作為硬化劑,只要是具有硬化環氧樹脂之機能者即可,並無特別限定,可舉例如酚系硬化劑、萘酚系硬化劑、活性酯系硬化劑、苯并噁嗪系硬化劑、氰酸酯系硬化劑、及碳二醯亞胺系硬化劑等。硬化劑係可1種單獨使用、或亦可併用2種以上。
作為酚系硬化劑及萘酚系硬化劑,就耐熱性及耐水性之觀點而言,以具有酚醛清漆構造之酚系硬化劑、或具有酚醛清漆構造之萘酚系硬化劑為較佳。又,就與導體層之密著性之觀點而言,以含氮酚系硬化劑為較佳,以含有三嗪骨架的酚系硬化劑為又較佳。其中,就使耐熱性、耐水性、及與導體層之密著性能高度地滿足之觀點而言,以含有三嗪骨架的苯酚酚醛清漆硬化劑為較佳。
作為酚系硬化劑及萘酚系硬化劑之具體例,可舉例如明和化成(股)製的「MEH-7700」、「MEH-7810」、「MEH-7851」、日本化藥(股)製的「NHN」、「CBN」、「GPH」、新日鐵住金(股)製的「SN170」、「SN180」、「SN190」、「SN475」、「SN485」、「SN495」、「SN-495V」「SN375」、「SN395」、DIC(股)製的「TD-2090」、「LA-7052」、「LA-7054」、「LA-1356」、「LA-3018-50P」、「EXB-9500」等。
作為活性酯系硬化劑並無特別限制,但一般較佳使用酚酯類、苯硫酚酯、N-羥基胺酯類、雜環羥基化
合物之酯類等的、在1分子中具有2個以上的反應活性為高的酯基之化合物。該活性酯系硬化劑係以藉由羧酸化合物及/或硫代羧酸化合物,與羥基化合物及/或硫醇化合物進行縮合反應而得到者為較佳。特別是就耐熱性提升之觀點而言,以由羧酸化合物與羥基化合物所得到之活性酯系硬化劑為較佳,以由羧酸化合物與酚化合物及/或萘酚化合物所得到之活性酯系硬化劑為又較佳。作為羧酸化合物,可舉例如苯甲酸、乙酸、琥珀酸、馬來酸、伊康酸、鄰苯二甲酸、間苯二甲酸、對苯二甲酸、焦蜜石酸等。作為酚化合物或萘酚化合物,可舉例如氫醌、間苯二酚、雙酚A、雙酚F、雙酚S、還原酚酞、甲基化雙酚A、甲基化雙酚F、甲基化雙酚S、苯酚、o-甲酚、m-甲酚、p-甲酚、兒茶酚、α-萘酚、β-萘酚、1,5-二羥基萘、1,6-二羥基萘、2,6-二羥基萘、二羥基苯甲酮、三羥基苯甲酮、四羥基苯甲酮、間苯三酚、苯三酚、雙環戊二烯型二酚化合物、苯酚酚醛清漆等。於此,所謂的「雙環戊二烯型二酚化合物」,係指在雙環戊二烯1分子中,2分子的酚進行縮合所得到之二酚化合物。
具體而言,以包含雙環戊二烯型二酚構造之活性酯化合物、包含萘構造之活性酯化合物、包含苯酚酚醛清漆的乙醯基化物之活性酯化合物、包含苯酚酚醛清漆的苯甲醯化物之活性酯化合物為較佳,其中,係以包含萘構造之活性酯化合物、包含雙環戊二烯型二酚構造之活性酯化合物為又較佳。所謂的「雙環戊二烯型二酚構造」係
表示由伸苯基-二環伸戊基-伸苯基所成之2價的構造單位。
作為活性酯系硬化劑的市售品,可舉出作為包含雙環戊二烯型二酚構造之活性酯化合物之「EXB9451」、「EXB9460」、「EXB9460S」、「HPC-8000-65T」、「HPC-8000H-65TM」、「EXB-8000L-65TM」(DIC(股)製)、作為包含萘構造之活性酯化合物之「EXB9416-70BK」(DIC(股)製)、作為包含苯酚酚醛清漆的乙醯基化物之活性酯化合物之「DC808」(三菱化學(股)製)、作為包含苯酚酚醛清漆的苯甲醯化物之活性酯化合物之「YLH1026」(三菱化學(股)製)、作為苯酚酚醛清漆的乙醯基化物之活性酯系硬化劑之「DC808」(三菱化學(股)製)、作為苯酚酚醛清漆的苯甲醯化物之活性酯系硬化劑之「YLH1026」(三菱化學(股)製)、「YLH1030」(三菱化學(股)製)、「YLH1048」(三菱化學(股)製)等。
作為苯并噁嗪系硬化劑之具體例,可舉出昭和高分子(股)製的「HFB2006M」、四國化成工業(股)製的「P-d」、「F-a」。
作為氰酸酯系硬化劑,可舉例如雙酚A二氰酸酯、多元酚氰酸酯、低聚(3-亞甲基-1,5-伸苯基氰酸酯)、4,4'-亞甲基雙(2,6-二甲基苯基氰酸酯)、4,4'-亞乙基二苯基二氰酸酯、六氟雙酚A二氰酸酯、2,2-雙(4-氰酸酯)苯基丙烷、1,1-雙(4-氰酸酯苯基甲烷)、雙(4-氰酸酯-3,5-二甲基苯基)甲烷、1,3-雙(4-氰酸酯苯基-1-(甲基亞乙
基))苯、雙(4-氰酸酯苯基)硫醚、及雙(4-氰酸酯苯基)醚等的2官能氰酸酯樹脂、由苯酚酚醛清漆及甲酚酚醛清漆等所衍生之多官能氰酸酯樹脂、該等氰酸酯樹脂一部分經三嗪化而得之預聚物等。作為氰酸酯系硬化劑之具體例,可舉出Lonza Japan(股)製的「PT30」及「PT60」(苯酚酚醛清漆型多官能氰酸酯樹脂)、「ULL-950S」(多官能氰酸酯樹脂)、「BA230」、「BA230S75」(雙酚A二氰酸酯之一部分或全部經三嗪化成為三聚體之預聚物)等。
作為碳二醯亞胺系硬化劑之具體例,可舉出日清紡Chemical(股)製的「V-03」、「V-07」等。
作為(B)成分,係以選自酚系硬化劑、萘酚系硬化劑、活性酯系硬化劑及氰酸酯系硬化劑之1種以上為較佳。又,就使樹脂組成物層之硬化物的萃取水導電率降低,且將樹脂組成物層之硬化物設置在高溫高濕度環境下時可抑制拉伸破壞強度之類的觀點而言,作為硬化劑係以耐熱穩定性為高者為較佳。作為耐熱穩定性為高的硬化劑,可舉出活性酯系硬化劑、氰酸酯系硬化劑、碳二醯亞胺系硬化劑等。就疎水性高、使樹脂組成物層之硬化物的萃取水導電率降低,且將樹脂組成物層之硬化物設置在高溫高濕度環境下時可抑制拉伸破壞強度之類的觀點而言,以選自活性酯系硬化劑及氰酸酯系硬化劑之1種以上為又較佳,以活性酯系硬化劑為更佳。
環氧樹脂與硬化劑之量比,就[環氧樹脂的環氧基的合計數]:[硬化劑的反應基的合計數]之比率計,以
1:0.01~1:2的範圍內為較佳,1:0.015~1:1.5為又較佳,1:0.02~1:1為更佳。於此,所謂的硬化劑的反應基係活性羥基、活性酯基等,依硬化劑之種類而有所不同。又,所謂的環氧樹脂的環氧基的合計數,係指對於全部的環氧樹脂而言,將各環氧樹脂的固形分質量除以環氧當量所得到的值進行合計而得到的值,所謂的硬化劑的反應基的合計數,係指對於全部的硬化劑而言,將各硬化劑的固形分質量除以反應基當量所得到的值進行合計而得到的值。藉由將環氧樹脂與硬化劑的量比設為上述範圍內,樹脂組成物層之硬化物之耐熱性可更加提升。
一實施形態中,樹脂組成物係包含先述之環氧樹脂及硬化劑。樹脂組成物,係以分別包含(A)作為環氧樹脂之液狀環氧樹脂與固體狀環氧樹脂之混合物(液狀環氧樹脂:固體狀環氧樹脂之質量比較佳為1:0.1~1:15,又較佳為1:0.3~1:12,更佳為1:0.6~1:10)、(B)作為硬化劑之選自酚系硬化劑、萘酚系硬化劑、活性酯系硬化劑及氰酸酯系硬化劑所成群之1種以上(較佳為選自活性酯系硬化劑及氰酸酯系硬化劑所成群之1種以上)為較佳。
樹脂組成物中之硬化劑的含有量並無特別限定,較佳為30質量%以下,又較佳為25質量%以下,更佳為20質量%以下。又,下限並無特別限制,以2質量%以上為較佳。
<(C)無機填充材>
一實施形態中,樹脂組成物亦可包含無機填充材。無機填充材之材料並無特別限定,可舉例如矽石、氧化鋁、玻璃、堇青石、矽氧化物、硫酸鋇、碳酸鋇、滑石、黏土、雲母粉、氧化鋅、水滑石、水鋁礦、氫氧化鋁、氫氧化鎂、碳酸鈣、碳酸鎂、氧化鎂、氮化硼、氮化鋁、氮化錳、硼酸鋁、碳酸鍶、鈦酸鍶、鈦酸鈣、鈦酸鎂、鈦酸鉍、氧化鈦、氧化鋯、鈦酸鋇、鈦鋯酸鋇、鋯酸鋇、鋯酸鈣、磷酸鋯、及磷鎢酸鋯等。該等之中,以矽石為特別適合。作為矽石,可舉例如無定形矽石、熔融矽石、結晶矽石、合成矽石、中空矽石等。又,作為矽石係以球狀矽石為較佳。無機填充材係可1種單獨使用,亦可組合2種以上來使用。
無機填充材的平均粒徑,就使無機填充材高填充並使薄膜絕緣性提升之觀點而言,以0.35μm以下為較佳,以0.32μm以下為又較佳,以0.3μm以下為更佳,以0.29μm以下為更又較佳。該平均粒徑之下限,就樹脂組成物層中之分散性提升之觀點而言,以0.05μm以上為較佳,以0.06μm以上為又較佳,以0.07μm以上為更佳。作為具有如此般的平均粒徑之無機填充材的市售品,可舉例如電氣化學工業(股)製「UFP-30」、新日鐵住金MATERIALS(股)製「SPH516-05」等。
無機填充材的平均粒徑係可藉由米氏(Mie)散射理論之雷射繞射‧散射法來進行測定。具體而言可藉由雷射繞射散射式粒度分布測定裝置,依體積基準來作成無
機填充材的粒度分布,並將其均粒徑作為平均粒徑來進行測定。測定樣品係可較佳使用為藉由超音波使無機填充材在甲基乙基酮中分散者。作為雷射繞射散射式粒度分布測定裝置,可使用(股)島津製作所製「SALD-2200」等。
無機填充材之比表面積,就降低後述之樹脂組成物層之最低熔融黏度之觀點而言,較佳為40m2/g以下,又較佳為37m2/g以下,更佳為33m2/g以下。該比表面積之下限,就樹脂組成物層之適當的黏彈性維持之觀點而言,較佳為1m2/g以上,又較佳為5m2/g以上,更佳為10m2/g、或15m2/g以上。比表面積係可使用例如BET全自動比表面積測定裝置(Mountech(股)製、Macsorb HM-1210)來進行測定。
無機填充材之真密度,就樹脂組成物層中之分散性提升之觀點而言,較佳為15g/cm3以下,又較佳為10g/cm3以下,更佳為5g/cm3以下。該真密度之下限,較佳為1g/cm3以上,又較佳為1.5g/cm3以上,更佳為2.0g/cm3以上。真密度係可使用例如超微比重計(Quantachrome Instruments Japan製、MUPY-21T)來進行測定。
無機填充材之比表面積(m2/g)與無機填充材之真密度(g/cm3)之乘積,以0.1~77為較佳,以26~77為又較佳,以30~70為更佳,以35~70為更又較佳。若該乘積為上述範圍內時,可使薄膜絕緣性提升。
無機填充材,就使耐濕性及分散性提高之觀
點而言,以經矽烷偶合劑、烷氧基矽烷化合物、及有機矽氮烷化合物等的至少1種的表面處理劑來進行表面處理為較佳。該等亦可為低聚物。作為表面處理劑之例,可舉出胺基矽烷系偶合劑、環氧基矽烷系偶合劑、巰基矽烷系偶合劑等的矽烷系偶合劑、烷氧基矽烷化合物、有機矽氮烷化合物、鈦酸酯系偶合劑等。作為表面處理劑之市售品,可舉例如信越化學工業(股)製「KBM403」(3-縮水甘油氧基丙基三甲氧基矽烷)、信越化學工業(股)製「KBM803」(3-巰基丙基三甲氧基矽烷)、信越化學工業(股)製「KBE903」(3-胺基丙基三乙氧基矽烷)、信越化學工業(股)製「KBM573」(N-苯基-3-胺基丙基三甲氧基矽烷)、信越化學工業(股)製「SZ-31」(六甲基二矽氮烷)、信越化學工業(股)製「KBM103」(苯基三甲氧基矽烷)、信越化學工業(股)製「KBM-4803」(長鏈環氧型矽烷偶合劑)等。表面處理劑係可1種類單獨使用,亦可組合2種類以上來使用。
藉由表面處理劑之表面處理的程度係可依無機填充材之每單位表面積的碳量來進行評估。無機填充材之每單位表面積的碳量,就無機填充材之分散性提升之觀點而言,以0.02mg/m2以上為較佳,以0.1mg/m2以上為又較佳,以0.2mg/m2以上為更佳。另一方面,就抑制樹脂清漆的熔融黏度及以薄片形態下的熔融黏度之上昇之觀點而言,以1mg/m2以下為較佳,以0.8mg/m2以下為又較佳,以0.5mg/m2以下為更佳。
無機填充材之每單位表面積的碳量,係可再將表面處理後之無機填充材藉由溶劑(例如、甲基乙基酮(MEK))進行洗淨處理後來測定。具體而言,除了將作為溶劑之充分的量的MEK用表面處理劑來進行表面處理之無機填充材外,另以25℃下超音波洗淨5分鐘。除去上清液,並使固形分乾燥後,可使用碳分析計來測定無機填充材之每單位表面積的碳量。作為碳分析計可使用(股)堀場製作所製「EMIA-320V」等。
樹脂組成物中之無機填充材的含有量(填充量),就使樹脂組成物層之厚度穩定性提升之觀點而言,將樹脂組成物中之不揮發成分設為100質量%時為50質量%以上,較佳為55質量%以上,又較佳為60質量%以上。樹脂組成物中之無機填充材的含有量之上限,就薄膜絕緣性之提升、以及絕緣層(樹脂組成物層之硬化物)之拉伸破壞強度之觀點而言,較佳為85質量%以下,又較佳為80質量%以下。
<(D)熱可塑性樹脂>
本發明之樹脂組成物係進而亦可含有(D)熱可塑性樹脂。
作為熱可塑性樹脂,可舉例如苯氧基樹脂、聚乙烯縮醛樹脂、聚烯烴樹脂、聚丁二烯樹脂、聚醯亞胺樹脂、聚醯胺醯亞胺樹脂、聚醚醯亞胺樹脂、聚碸樹脂、聚醚碸樹脂、聚苯醚樹脂、聚碳酸酯樹脂、聚醚醚酮樹
脂、聚酯樹脂,以苯氧基樹脂為較佳。熱可塑性樹脂係可1種單獨使用、或亦可組合2種以上來使用。
熱可塑性樹脂之聚苯乙烯換算的重量平均分子量係以8,000~70,000的範圍內為較佳,以10,000~60,000的範圍內為又較佳,以20,000~60,000的範圍內為更佳。熱可塑性樹脂之聚苯乙烯換算的重量平均分子量係可用凝膠滲透層析法(GPC)法來進行測定。具體而言,熱可塑性樹脂之聚苯乙烯換算的重量平均分子量係可使用作為測定裝置之(股)島津製作所製LC-9A/RID-6A、作為管柱之昭和電工(股)製Shodex K-800P/K-804L/K-804L、作為移動相之三氯甲烷等,以40℃下測定管柱溫度,並使用標準聚苯乙烯的檢量線來算出。
作為苯氧基樹脂,可舉例如具有選自雙酚A骨架、雙酚F骨架、雙酚S骨架、雙酚苯乙酮骨架、酚醛清漆骨架、聯苯骨架、茀骨架、雙環戊二烯骨架、降莰烯骨架、萘骨架、蒽骨架、金剛烷骨架、萜烯骨架、及三甲基環己烷骨所成群之1種以上的骨架之苯氧基樹脂。苯氧基樹脂的末端亦可是酚性羥基、環氧基等之任一的官能基皆可。苯氧基樹脂係可1種單獨使用,亦可組合2種以上來使用。作為苯氧基樹脂之具體例,可舉出三菱化學(股)製的「1256」及「4250」(皆為含有雙酚A骨架的苯氧基樹脂)、「YX8100」(含有雙酚S骨架的苯氧基樹脂)、及「YX6954」(含有雙酚苯乙酮骨架的苯氧基樹脂),其他亦可舉出新日鐵住金化學(股)製的「FX280」及「FX293」、
三菱化學(股)製的「YX6954BH30」、「YX7553」、「YX7553BH30」、「YL7769BH30」、「YL6794」、「YL7213」、「YL7290」及「YL7482」等。
作為聚乙烯縮醛樹脂,可舉例如聚乙烯甲醛樹脂、聚乙烯丁醛樹脂,以聚乙烯丁醛樹脂為較佳。作為聚乙烯縮醛樹脂之具體例,可舉例如電氣化學工業(股)製的「電化butyral 4000-2」、「電化butyral 5000-A」、「電化butyral 6000-C」、「電化butyral 6000-EP」、積水化學工業(股)製的S-LecBH系列、BX系列(例如BX-5Z)、KS系列(例如KS-1)、BL系列、BM系列等。
作為聚醯亞胺樹脂之具體例,可舉出新日本理化(股)製的「RIKA COAT SN20」及「RIKA COAT PN20」。作為聚醯亞胺樹脂之具體例又可舉出使2官能性羥基末端的聚丁二烯、二異氰酸酯化合物及四元酸酐進行反應而得到之線狀聚醯亞胺(日本特開2006-37083號公報記載的聚醯亞胺)、含有聚矽氧烷骨架之聚醯亞胺(日本特開2002-12667號公報及日本特開2000-319386號公報等記載的聚醯亞胺)等的變性聚醯亞胺。
作為聚醯胺醯亞胺樹脂之具體例,可舉出東洋紡績(股)製的「VYLOMAX HR11NN」及「VYLOMAX HR16NN」。作為聚醯胺醯亞胺樹脂之具體例,又可舉出日立化成工業(股)製的「KS9100」、「KS9300」(含有聚矽氧烷骨架之聚醯胺醯亞胺)等的變性聚醯胺醯亞胺。
作為聚醚碸樹脂之具體例,可舉出住友化學
(股)製的「PES5003P」等。
作為聚碸樹脂之具體例,可舉出Solvay Advanced Polymers(股)製的聚碸「P1700」、「P3500」等。
其中,作為熱可塑性樹脂以苯氧基樹脂、聚乙烯縮醛樹脂為較佳。因此,在適合的一實施形態中,熱可塑性樹脂係包含選自苯氧基樹脂及聚乙烯縮醛樹脂所成群之1種以上。
若樹脂組成物為含有熱可塑性樹脂之情形時,熱可塑性樹脂的含有量較佳為0.5質量%~10質量%,又較佳為0.6質量%~5質量%,更佳為0.7質量%~3質量%。
<(E)硬化促進劑>
本發明之樹脂組成物係進而亦可含有(E)硬化促進劑。
作為硬化促進劑,可舉例如磷系硬化促進劑、胺系硬化促進劑、咪唑系硬化促進劑、胍系硬化促進劑、金屬系硬化促進劑、有機過氧化物系硬化促進劑等,以磷系硬化促進劑、胺系硬化促進劑、咪唑系硬化促進劑、金屬系硬化促進劑為較佳,以胺系硬化促進劑、咪唑系硬化促進劑、金屬系硬化促進劑為又較佳。硬化促進劑係可1種單獨使用,亦可組合2種以上來使用。
作為磷系硬化促進劑,可舉例如三苯基膦、
硼酸鏻化合物、四苯基鏻四苯基硼酸酯、n-丁基鏻四苯基硼酸酯、四丁基鏻癸酸鹽、(4-甲基苯基)三苯基鏻硫氰酸酯、四苯基鏻硫氰酸酯、丁基三苯基鏻硫氰酸酯等,以三苯基膦、四丁基鏻癸酸鹽為較佳。
作為胺系硬化促進劑,可舉例如三乙基胺、三丁基胺等的三烷基胺、4-二甲基胺吡啶、苄基二甲基胺、2,4,6,-參(二甲基胺基甲基)酚、1,8-二氮雜雙環(5,4,0)-十一烯等,以4-二甲基胺吡啶、1,8-二氮雜雙環(5,4,0)-十一烯為較佳。
作為咪唑系硬化促進劑,可舉例如2-甲基咪唑、2-十一烷基咪唑、2-十七烷基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、1,2-二甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、2-苯基-4-甲基咪唑、1-苄基-2-甲基咪唑、1-苄基-2-苯基咪唑、1-氰乙基-2-甲基咪唑、1-氰乙基-2-十一烷基咪唑、1-氰乙基-2-乙基-4-甲基咪唑、1-氰乙基-2-苯基咪唑、1-氰乙基-2-烷基咪唑偏苯三甲酸鹽、1-氰乙基-2-苯基咪唑偏苯三甲酸鹽、2,4-二胺基-6-[2'-甲基咪唑基-(1')]-乙基-s-三嗪、2,4-二胺基-6-[2'-十一烷基咪唑-(1')]-乙基-s-三嗪、2,4-二胺基-6-[2'-乙基-4'-甲基咪唑基-(1')]-乙基-s-三嗪、2,4-二胺基-6-[2'-甲基咪唑基-(1')]-乙基-s-三嗪異氰脲酸加成物、2-苯基咪唑異氰脲酸加成物、2-苯基-4,5-二羥甲基咪唑、2-苯基-4-甲基-5-羥甲基咪唑、2,3-二氫-1H-吡咯[1,2-a]苯并咪唑、1-十二烷基-2-甲基-3-苄基咪唑鎓氯化物、2-甲基咪唑啉、2-苯基咪唑啉等
的咪唑化合物及咪唑化合物與環氧樹脂的加成物,以2-乙基-4-甲基咪唑、1-苄基-2-苯基咪唑為較佳。
作為咪唑系硬化促進劑,亦可使用市售品可舉例如三菱化學(股)製的「P200-H50」等。
作為胍系硬化促進劑,可舉例如二氰二胺、1-甲基胍、1-乙基胍、1-環己基胍、1-苯基胍、1-(o-甲苯基)胍、二甲基胍、二苯基胍、三甲基胍、四甲基胍、五甲基胍、1,5,7-三氮雜雙環[4.4.0]癸-5-烯、7-甲基-1,5,7-三氮雜雙環[4.4.0]癸-5-烯、1-甲基雙胍、1-乙基雙胍、1-n-丁基雙胍、1-n-十八烷基雙胍、1,1-二甲基雙胍、1,1-二乙基雙胍、1-環己基雙胍、1-烯丙基雙胍、1-苯基雙胍、1-(o-甲苯基)雙胍等,以二氰二胺、1,5,7-三氮雜雙環[4.4.0]癸-5-烯為較佳。
作為金屬系硬化促進劑,可舉例如鈷、銅、鋅、鐵、鎳、錳、錫等的金屬之有機金屬錯合物或有機金屬鹽。作為有機金屬錯合物之具體例,可舉出乙醯丙酮酸鈷(II)、乙醯丙酮酸鈷(III)等的有機鈷錯合物、乙醯丙酮酸銅(II)等的有機銅錯合物、乙醯丙酮酸鋅(II)等的有機鋅錯合物、乙醯丙酮酸鐵(III)等的有機鐵錯合物、乙醯丙酮酸鎳(II)等的有機鎳錯合物、乙醯丙酮酸錳(II)等的有機錳錯合物等。作為有機金屬鹽,可舉例如辛酸鋅、辛酸錫、環烷酸鋅、環烷酸鈷、硬脂酸錫、硬脂酸鋅等。
作為有機過氧化物系硬化促進劑,可舉例如過氧化二異丙苯、過氧化環己酮、tert-丁基過氧化苯甲酸酯、甲基
乙基酮過氧化物、過氧化二異丙苯、tert-丁基過氧化異丙苯、二-tert-丁基過氧化物、過氧化氫二異丙苯、過氧化氫異丙苯、tert-丁基氫過氧化物等。作為有機過氧化物系硬化促進劑,係可使用市售品可舉例如日油公司製的「PERCUMYL D」等。
樹脂組成物中之硬化促進劑的含有量並無特別限定,將環氧樹脂與硬化劑之不揮發成分設為100質量%時,以0.01質量%~3質量%為較佳。
<(F)耐燃劑>
本發明之樹脂組成物係進而亦可包含(F)耐燃劑。作為耐燃劑,可舉例如有機磷系耐燃劑、含有機系氮的磷化合物、氮化合物、聚矽氧系耐燃劑、金屬氫氧化物等。耐燃劑係可1種單獨使用、或亦可併用2種以上。
作為耐燃劑亦可使用市售品,可舉例如三光(股)製的「HCA-HQ」、大八化學工業(股)製的「PX-200」等。作為耐燃劑以不易水解者為較佳,例如以10-(2,5-羥基苯基)-10-氫-9-氧雜-10-磷雜菲-10-氧化物等為較佳。
若樹脂組成物含有耐燃劑之情形時,耐燃劑的含有量並無特別限定,較佳為0.5質量%~20質量%,又較佳為0.5質量%~15質量%,更佳為0.5質量%~10質量%為更較佳。
<(G)有機填充材>
樹脂組成物,就使樹脂組成物層之硬化物之拉伸破壞強度提升之觀點而言,亦可包含(G)有機填充材。作為有機填充材,可使用在形成印刷配線板之絕緣層之際能夠使用之任意的有機填充材,可舉例如橡膠粒子、聚醯胺微粒子、聚矽氧粒子等。
作為橡膠粒子亦可使用市售品,可舉例如Dow Chemical日本(股)製的「EXL2655」、Aica工業(股)製的「AC3401N」、「AC3816N」等。
作為橡膠粒子,就離子性為低、可使樹脂組成物層之硬化物之萃取水導電率降低之觀點而言,以例如Aica工業(股)製的「AC3816N」、「AC3401N」等為較佳。
若樹脂組成物含有機填充材之情形時,有機填充材的含有量較佳為0.1質量%~20質量%,又較佳為0.2質量%~10質量%,更佳為0.3質量%~5質量%、或0.5質量%~3質量%。
<(H)其他添加劑>
樹脂組成物係進而因應所需亦可包含其他添加劑,作為上述之其他的添加劑,可舉例如有機銅化合物、有機鋅化合物及有機鈷化合物等的有機金屬化合物、以及增稠劑、消泡劑、調平劑、密著性賦予劑、及著色劑等的樹脂添加劑等。
本發明之樹脂薄片係可產生薄膜絕緣性為優異之絕緣層(樹脂組成物層之硬化物)。因此,本發明之樹脂薄片係可適合使用作為用於形成印刷配線板之絕緣層(印刷配線板之絕緣層形成用)的樹脂薄片,且可更適合使用作為用於形成印刷配線板之層間絕緣層之樹脂薄片(印刷配線板之層間絕緣層用樹脂薄片)。又,例如在具備有第1導體層、第2導體層、與設置在第1導體層及第2導體層之間之絕緣層之印刷配線板中,因藉由本發明之樹脂薄片而形成絕緣層,故可將第1及第2導體層之間的絕緣層之厚度設為6μm以下(較佳為5.5μm以下,又較佳為5μm以下),同時可成為絕緣性能為優異。適合的一實施形態中,本發明之樹脂薄片,其係包含第1導體層、第2導體層、與絕緣第1導體層和第2導體層的絕緣層、且第1導體層和第2導體層之間的絕緣層之厚度為6μm以下的印刷配線板之絕緣層形成用。
[樹脂薄片]
本發明之樹脂薄片係具備有支撐體、與設置在該支撐體上之樹脂組成物層、且樹脂組成物層係由樹脂組成物所形成。
樹脂組成物層之厚度,就印刷配線板之薄型化之觀點而言,較佳為15μm以下,又較佳為12μm以下,更佳為10μm以下,更又較佳為8μm以下。樹脂組成物層之厚度之下限,並無特別限定,通常可設為1μm以
上、1.5μm以上、2μm以上等。
作為支撐體,可舉例如由塑膠材料所成之薄片、金屬箔、脫模紙,以由塑膠材料所成之薄片、金屬箔為較佳。
若使用由塑膠材料所成之薄片來作為支撐體之情形時,作為塑膠材料可舉例如聚對苯二甲酸乙二酯(以下有時簡稱為「PET」)、聚萘二甲酸乙二酯(以下有時簡稱為「PEN」)等的聚酯、聚碳酸酯(以下簡稱為「PC」)、聚甲基丙烯酸甲酯(PMMA)等的丙烯酸、環狀聚烯烴、三乙醯基纖維素(TAC)、聚醚硫醚(PES)、聚醚酮、聚醯亞胺等。其中,以聚對苯二甲酸乙二酯、聚萘二甲酸乙二酯為較佳,以便宜的聚對苯二甲酸乙二酯為特佳。
若使用金屬箔來作為支撐體之情形時,作為金屬箔可舉例如銅箔、鋁箔等,以銅箔為較佳。作為銅箔,可使用由銅的單金屬所成的箔,亦可使用由銅與其他金屬(例如錫、鉻、銀、鎂、鎳、鋯、矽、鈦等)的合金所成的箔。
支撐體係亦可對於與樹脂組成物層接合之面施予拋光處理、電暈處理、帶電防止處理。
又,作為支撐體係亦可使用在與樹脂組成物層接合之面上具有脫模層之附脫模層之支撐體。作為使用於附脫模層之支撐體之脫模層之脫模劑,可舉例如選自醇酸樹脂、聚烯烴樹脂、胺甲酸乙酯樹脂、及聚矽氧樹脂所
成群之1種以上的脫模劑。附脫模層之支撐體亦可使用市售品,例如具有將醇酸樹脂系脫模劑作為主成分之脫模層之PET薄片,可舉出Lintec(股)製的「SK-1」、「AL-5」、「AL-7」、Toray(股)製「Lumirror T6AM」、「Lumirror R80」等。
作為支撐體之厚度並無特別限定,但以5μm~75μm的範圍內為較佳,10μm~60μm的範圍內為又較佳。尚,若使用附脫模層之支撐體之情形時,以附脫模層之支撐體全體之厚度為上述範圍內為較佳。
樹脂薄片係可藉由例如調製將樹脂組成物溶解在有機溶劑中之樹脂清漆,並使用模塗布機等將該樹脂清漆塗布在支撐體上,進而藉由使其進行乾燥使得樹脂組成物層形成從而製造。
作為有機溶劑,可舉例如丙酮、甲基乙基酮(MEK)及環己酮等的酮類、乙酸乙酯、乙酸丁酯、乙酸溶纖劑、丙二醇單甲基醚乙酸酯及卡必醇乙酸酯等的乙酸酯類、溶纖劑及丁基卡必醇等的卡必醇類、甲苯及二甲苯等的芳香族烴類、二甲基甲醯胺、二甲基乙醯胺(DMAc)及N-甲基吡咯啶酮等的醯胺系溶劑等。有機溶劑係可以1種單獨使用,亦可組合2種以上來使用。
乾燥係可藉由加熱、吹熱風等的周知的方法來進行實施。乾燥條件並無特別限定,若樹脂組成物層中之有機溶劑的含有量為10質量%以下時,較佳以成為5質量%以下之方式來使其乾燥。依樹脂清漆中之有機溶劑
的沸點而有所不同,例如若使用包含30質量%~60質量%的有機溶劑之樹脂清漆之情形時,藉由以50℃~150℃下使其乾燥3分鐘~10分鐘乾燥,從而可形成樹脂組成物層。
樹脂薄片中,在未與樹脂組成物層之支撐體接合之面上(即,與支撐體為相反側之面),可進而層合以支撐體為基準的保護薄片。保護薄片之厚度並無特別限定,例如為1μm~40μm。藉由層合保護薄片,可防止對於樹脂組成物層的表面之灰塵等的附著或損傷。樹脂薄片係可以捲成輥狀來做保存。若樹脂薄片具有保護薄片之情形時,藉由將保護薄片剝下而可以使用。
樹脂薄片中之樹脂組成物層之最低熔融黏度,就可得到良好的配線埋置性之觀點而言,較佳為12000poise(1200Pa‧s)以下,又較佳為10000poise(1000Pa‧s)以下,更佳為8000poise(800Pa‧s)以下、5000poise(500Pa‧s)以下、或4000poise(400Pa‧s)以下。該最低熔融黏度之下限,就即便是樹脂組成物層薄能將厚度穩定並維持之觀點而言,以1000poise(100Pa‧s)以上為較佳,以1500poise(150Pa‧s)以上為又較佳,以2000poise(200Pa‧s)以上為更佳。
所謂的樹脂組成物層之最低熔融黏度,係指於樹脂組成物層的樹脂熔融時,樹脂組成物層所呈現之最低黏度。詳細而言,以一定的昇溫速度加熱樹脂組成物層並使樹脂熔融時,初期的階段係熔融黏度為溫度上昇的同
時降低,之後若超過一定程度時,溫度上昇的同時熔融黏度為上昇。所謂的最低熔融黏度,係指上述極小點之熔融黏度。樹脂組成物層之最低熔融黏度係可藉由動態黏彈性法來進行測定,例如可根據後述之<最低熔融黏度之測定>所記載之方法來進行測定。
[硬化物]
使本發明之樹脂薄片之樹脂組成物層熱硬化所得到之硬化物,係滿足特定的萃取水導電率(特性1)及特定的拉伸破壞強度之比(特性2)之中至少一者。依據本發明,藉由樹脂組成物層之硬化物滿足如下述般的特性,從而可產生薄層絕緣性為優異之絕緣層。
(特性1)樹脂組成物層之硬化物在120℃下20小時之萃取水導電率A為50μS/cm以下、且樹脂組成物層之硬化物在160℃下20小時之萃取水導電率B為200μS/cm以下。
(特性2)樹脂組成物層之硬化物且厚度為10μm之硬化物之HAST試驗後之拉伸破壞強度B,對樹脂組成物層之硬化物且厚度為10μm之硬化物之拉伸破壞強度A之比(B/A)為0.65以上1以下。
滿足特性1之樹脂組成物層之硬化物,作為樹脂組成物中所包含之成分(例如環氧樹脂及硬化劑等),使用純度為高的樹脂、使用不易水解的樹脂、或使用耐熱性為高的樹脂,藉由調整無機填充材的量而能夠實現。
滿足特性2之樹脂組成物層之硬化物,作為樹脂組成物中所包含之成分(例如環氧樹脂及硬化劑等),使用純度為高的樹脂、使用不易水解的樹脂、或使用耐熱性為高的樹脂,藉由調整無機填充材的量而能夠實現。
本發明中,只要樹脂組成物層之硬化物能滿足特性1及特性2中任一者,即可賦予薄膜絕緣性為優異的絕緣層,但具有特性1及特性2兩者之樹脂組成物層之硬化物,係因為可產生薄膜絕緣性更加優異的絕緣層,故為較佳。
本發明之樹脂薄片之樹脂組成物層之熱硬化條件並無特別限定,可使用例如於形成後述之印刷配線板之絕緣層時通常被採用之條件。又,亦可於使樹脂組成物熱硬化前進行予備加熱,且熱硬化條件中之加熱係亦可包含予備加熱在內進行多次。作為熱硬化條件之一例,首先將樹脂組成物以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下90分鐘來使其熱硬化。
本發明之樹脂薄片之樹脂組成物層之硬化物(例如將樹脂組成物層以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下90分鐘來使其熱硬化而得到之硬化物)在120℃下20小時的萃取水導電率A,就可產生薄膜絕緣性為優異之絕緣層之觀點而言為50μS/cm以下,且該樹脂組成物層之硬化物在160℃下20小時的萃取水導電率B為200μS/cm。萃取水導電率A係以47μS/cm以下為較佳,以45μS/cm以下為又較佳,以
43μS/cm以下為更佳。萃取水導電率B,就可產生薄膜絕緣性為優異之絕緣層之觀點而言,以195μS/cm以下為較佳,以190μS/cm以下為較佳,以185μS/cm以下為又較佳。樹脂組成物層之硬化物在120℃下20小時之萃取水導電率A及樹脂組成物層之硬化物在160℃下20小時之萃取水導電率B,係可根據例如後述之<硬化物之萃取水導電率之測定>所記載之方法來進行測定。
本發明之樹脂薄片之樹脂組成物層之硬化物(例如將樹脂組成物層以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下90分鐘來使其熱硬化而得到之硬化物)的玻璃移轉溫度(DMA),就使樹脂組成物層之硬化物之萃取水導電率降低、且將樹脂組成物層之硬化物配置在高溫高濕度環境下時可抑制拉伸破壞強度之降低之觀點而言,以160℃以上為較佳為,以170℃以上為又較佳,以180℃以上為更佳。樹脂組成物層之硬化物的玻璃移轉溫度,係可依據例如<硬化物之玻璃移轉溫度之測定>所記載之方法來進行測定。
本發明之樹脂薄片之樹脂組成物層之硬化物(例如將樹脂組成物層以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下90分鐘來使其熱硬化而得到之硬化物)且厚度為10μm之硬化物之拉伸破壞強度A,就可產生薄膜絕緣性為優異之絕緣層之觀點而言,以50MPa以上為較佳,以60MPa以上為又較佳,以70MPa以上為更佳。拉伸破壞強度A之上限值並無特別限定,可
設為150MPa以下、140以下、130MPa以下、120MPa以下、110MPa以下等。
本發明之樹脂薄片之樹脂組成物層之硬化物且厚度為10μm之硬化物(例如將樹脂組成物層以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下90分鐘來使其熱硬化而得到之硬化物)之HAST試驗後之拉伸破壞強度B,就可得到薄膜絕緣性為優異之絕緣層之觀點而言,以50MPa以上為較佳,以55MPa以上為又較佳,以60MPa以上為更佳,以70MPa以上為更又較佳。拉伸破壞強度B之上限值並無特別限定,可設為150MPa以下、140以下、130MPa以下、120MPa以下、110MPa以下等。本發明中,HAST((Highly Accelerated temperature and humidity Stress Test)試驗係可藉由使用例如高度加速壽命試驗裝置(ETAC製「PM422」),將樹脂組成物層之硬化物以130℃下85%的相對濕度之條件使其經過100小時來實行。
本發明中,拉伸破壞強度B對拉伸破壞強度A之比(B/A),就可產生薄膜絕緣性為優異之絕緣層之觀點而言,以0.65以上為較佳,以0.68以上為又較佳,以0.70以上為更佳。又,拉伸破壞強度B對拉伸破壞強度A之比(B/A),就可產生薄膜絕緣性為優異之絕緣層之觀點而言,以1以下為較佳,以0.9以下為又較佳,以0.8以下為更佳。
本發明之樹脂薄片之樹脂組成物層之硬化物
且厚度為10μm之硬化物之拉伸破壞強度A及厚度為10μm之硬化物之HAST試驗後之拉伸破壞強度B,係可根據例如後述之<硬化物之拉伸破壞強度之測定>所記載之方法來進行測定,並可使用藉由該測定所得到之測定值來算出拉伸破壞強度B對拉伸破壞強度A之比(B/A)。
使本發明之樹脂薄片之樹脂組成物層熱硬化而得到之硬化物(例如將樹脂組成物以100℃下30分鐘,接下來,以175℃下30分鐘使其熱硬化而得到之硬化物),即使在130℃、85RH%、外加3.3V之環境下經過100小時後,亦可展現出良好的絕緣電阻值。即,產生展現出良好的絕緣電阻值之絕緣層。該絕緣電阻值之上限,較佳為1012Ω以下,又較佳為1011Ω以下,更佳為1010Ω以下。對於下限並無特別限定,但較佳為106Ω以上,又較佳為107Ω以上。絕緣電阻值之測定,係可根據後述之<絕緣可靠性之評估、導體層之間的絕緣層之厚度之測定>所記載之方法來進行測定。
本發明中亦包含硬化物,其係樹脂組成物層之硬化物,在120℃下20小時的萃取水導電率A為50μS/cm以下,且在160℃下20小時的萃取水導電率B為200μS/cm以下之硬化物。硬化物係與本發明之樹脂薄片之樹脂組成物層之硬化物為相同之構成。又用於形成硬化物之樹脂組成物之硬化條件,係與樹脂薄片之硬化條件為相同。本發明之硬化物(例如將樹脂組成物層以100℃下30分鐘,接下來,以175℃下30分鐘,進而以190℃下
90分鐘來使其熱硬化而得到之硬化物)中,萃取水導電率A之較佳範圍及萃取水導電率B之較佳範圍,係與上述之樹脂薄片之硬化物為相同。對於除了萃取水導電率以外之硬化物之物性值(玻璃移轉溫度、拉伸破壞強度A、拉伸破壞強度B、拉伸破壞強度B對拉伸破壞強度A之比(B/A)及絕緣電阻值)之較佳範圍,亦與上述之樹脂薄片之硬化物為相同。
[印刷配線板、印刷配線板之製造方法]
本發明之印刷配線板係包含藉由本發明之樹脂薄片之樹脂組成物層之硬化物所形成之絕緣層、第1導體層、及第2導體層。本發明之印刷配線基板係亦可以是具備有本發明之硬化物來作為絕緣層。絕緣層係被設置在第1導體層和第2導體層之間,而來絕緣第1導體層和第2導體層(導體層亦稱為配線層)。藉由本發明之樹脂薄片之樹脂組成物層之硬化物所形成之絕緣層,因為薄膜絕緣性為優異,故即便是第1及第2導體層之間的絕緣層之厚度為6μm以下絕緣性亦為優異。
第1及第2導體層之間的絕緣層之厚度,較佳為6μm以下,又較佳為5.5μm以下,更佳為5μm以下。對於下限並無特別限定,可設為0.1μm以上。所謂的第1及第2導體層之間的絕緣層之厚度,如於圖1表示之一例般,係指第1導體層5之主面51與第2導體層6之主面61之間的絕緣層7之厚度t1。第1及第2導體層係
介隔著絕緣層並相鄰之導體層,主面51及主面61係相互相向。第1及第2導體層之間的絕緣層之厚度,係可根據後述之<絕緣可靠性之評估、導體層之間的絕緣層之厚度之測定>所記載之方法來進行測定。
尚,絕緣層全體之厚度t2,較佳為20μm以下,又較佳為15μm以下,更佳為12μm以下。對於下限並無特別限定,可設為1μm以上。
本發明之印刷配線板係可使用上述之樹脂薄片,並藉由包含下述(I)及(II)之步驟之方法來製造。
(I)在內層基板上,以樹脂薄片之樹脂組成物層與內層基板接合之方式來進行層合之步驟
(II)將樹脂組成物層熱硬化來形成絕緣層之步驟
所謂的步驟(I)中使用之「內層基板」,係主要指玻璃環氧基板、金屬基板、聚酯基板、聚醯亞胺基板、BT樹脂基板、熱硬化型聚苯醚基板等的基板、或在該基板的單面或雙面上形成經圖型加工之導體層(電路)之電路基板。又,於製造印刷配線板時,進而應該形成絕緣層及/或導體層之中間製造物之內層電路基板,亦包含在本發明中所言及之「內層基板」中。印刷配線板為零件內附電路板之情形時,可使用內附零件之內層基板。
內層基板與樹脂薄片之層合,係可藉由例如從支撐體側將樹脂薄片加熱壓黏在內層基板上來進行。作為將樹脂薄片加熱壓黏在內層基板上之構件(以下亦稱為「加熱壓黏構件」),可舉例如經加熱的金屬板(SUS鏡板
等)或金屬輥(SUS輥)等。尚,並非將加熱壓黏構件直接壓製在樹脂薄片上,而是使樹脂薄片可充分地追隨內層基板的表面凹凸,以介隔著耐熱橡膠等的彈性材來進行壓製為較佳。
內層基板與樹脂薄片之層合係可藉由真空層合法來實施。真空層合法中,加熱壓黏溫度較佳為60℃~160℃,又較佳為80℃~140℃的範圍內,加熱壓黏壓力較佳為0.098MPa~1.77MPa,又較佳為0.29MPa~1.47MPa的範圍內,加熱壓黏時間較佳為20秒鐘~400秒鐘,又較佳為30秒鐘~300秒鐘的範圍內。層合係較佳以壓力26.7hPa以下之減壓條件下來實施。
層合係可藉由市售的真空貼合機來進行。作為市售的真空貼合機,可舉例如(股)名機製作所製的真空加壓式貼合機、Nikko-materials(股)製的真空貼合機等。
於層合後,在常壓下(大氣壓下),藉由例如從支撐體側來壓製加熱壓黏構件,從而可進行經層合的樹脂薄片之平滑化處理。平滑化處理之壓製條件,係可設定與上述層合之加熱壓黏條件為相同之條件。平滑化處理係可藉由市售的貼合機來進行。尚,層合與平滑化處理係可使用上述之市售的真空貼合機來連續的進行。
支撐體係可於步驟(I)與步驟(II)之間除去,亦可於步驟(II)之後除去。
步驟(II)中,將樹脂組成物層熱硬化來形成絕緣層。
樹脂組成物層之熱硬化條件並特別限定,可使用於形成印刷配線板之絕緣層時,通常所採用之條件。
例如樹脂組成物層之熱硬化條件,係依樹脂組成物的種類等而有所不同,可設硬化溫度為120℃~240℃的範圍內(較佳為150℃~220℃的範圍內,又較佳為170℃~200℃的範圍內),硬化時間為5分鐘~120分鐘的範圍內(較佳為10分鐘~100分鐘,又較佳為15分鐘~90分鐘)。
使樹脂組成物層熱硬化前,可將樹脂組成物層藉以低於硬化溫度之溫度來進行予備加熱。例如可在使樹脂組成物層熱硬化之前,藉以50℃以上未滿120℃(較佳為60℃以上110℃以下,又較佳為70℃以上100℃以下)的溫度,將樹脂組成物層進行予備加熱5分鐘以上(較佳為5分鐘~150分鐘,又較佳為15分鐘~120分鐘)。
於製造印刷配線板時,進而可實施(III)在絕緣層上穿孔之步驟、(IV)將絕緣層進行粗化處理之步驟、(V)形成導體層之步驟。該等的步驟(III)~(V)係可根據被用在印刷配線板之製造中業者所周知之各種方法來實施即可。尚,若於步驟(II)後除去支撐體之情形時,該支撐體之除去係可於步驟(II)與步驟(III)之間、步驟(III)與步驟(IV)之間、或步驟(IV)與步驟(V)之間來實施。又,因應所需亦可反覆實施步驟(II)~(V)之絕緣層及導體層之形成,來形成多層配線板。此情形時,分別的導體層之間的絕緣層之厚度(圖1的t1)係以上述範圍內為較佳。
步驟(III)係在絕緣層上穿孔之步驟,據此,在絕緣層上可形成通孔洞、穿通孔等的孔洞。步驟(III)係因應於絕緣層之形成所使用之樹脂組成物的組成等,可使用例如鑽孔、雷射、等離子等來實施。孔洞的尺寸或形狀係可因應印刷配線板之設計來適當決定。
步驟(IV)係將絕緣層進行粗化處理之步驟。粗化處理之程序、條件並無特別限定,可採用形成印刷配線板之絕緣層時通常所使用的周知的程序、條件。可依此順序實施例如藉由膨潤液之膨潤處理、藉由氧化劑之粗化處理、藉由中和液之中和處理,來將絕緣層進行粗化處理。作為膨潤液並無特別限定,可舉出鹼溶液、界面活性劑溶液等,較佳為鹼溶液,作為該鹼溶液,以氫氧化鈉溶液、氫氧化鉀溶液為又較佳。作為目前市售之膨潤液,可舉例如Atotech Japan(股)製的「Swelling Dip Securiganth P」、「Swelling Dip Securiganth SBU」等。藉由膨潤液之膨潤處理並無特別限定,例如可將絕緣層在30℃~90℃的膨潤液中浸漬1分鐘~20分鐘來進行。就能將絕緣層的樹脂之膨潤抑制在適當的程度之觀點而言,以使絕緣層在40℃~80℃的膨潤液中浸漬5分鐘~15分鐘為較佳。作為氧化劑並無特別限定,可舉例如將過錳酸鉀或過錳酸鈉溶解在氫氧化鈉的水溶液之鹼性過錳酸溶液。藉由鹼性過錳酸溶液等的氧化劑之粗化處理,以使絕緣層在加熱至60℃~80℃的氧化劑溶液中,浸漬10分鐘~20分鐘來進行為較佳。又,鹼性過錳酸溶液之過錳酸鹽的濃度係以5質量
%~10質量%為較佳。作為目前市售之氧化劑,可舉例如Atotech Japan(股)製的「concentrate Compact CP」、「Swelling Dip Securiganth P」等的鹼性過錳酸溶液。又,作為中和液係以酸性的水溶液為較佳,作為市售品,可舉例如Atotech Japan(股)製的「Reduction solution Securiganth P」。藉由中和液之處理係可將未藉由氧化劑之粗化處理的處理面,在30℃~80℃的中和液中浸漬5分鐘~30分鐘來進行。就作業性等的觀點而言,以將未藉由氧化劑之粗化處理的對象物,在40℃~70℃的中和液中浸漬5分鐘~20分鐘之方法為較佳。
一實施形態中,粗化處理後的絕緣層表面之算術平均粗度Ra,較佳為400nm以下,又較佳為350nm以下,更佳為300nm以下、250nm以下、200nm以下、150nm以下、或100nm以下。絕緣層表面之算術平均粗度(Ra)亦可使用非接觸型表面粗度計來進行測定。作為非接觸型表面粗度計之具體例,可舉出Veeco Instruments公司製的「WYKO NT3300」。
步驟(V)係形成導體層之步驟。若在內層基板上未形成導體層之情形時,步驟(V)為形成第1的導體層之步驟,若在內層基板上有形成導體層之情形時,該導體層為第1導體層、且步驟(V)為形成第2的導體層之步驟。
導體層中使用之導體材料並無特別限定。適合的實施形態中,導體層係包含選自金、鉑、鈀、銀、
銅、鋁、鈷、鉻、鋅、鎳、鈦、鎢、鐵、錫及銦所成群之1種以上的金屬。導體層可以是單金屬層,亦可以是合金層,作為合金層,可舉出由例如選自上述之群之2種以上的金屬的合金(例如鎳‧鉻合金、銅‧鎳合金及銅‧鈦合金)所形成之層。其中,就導體層形成之汎用性、成本、圖型化之容易性等的觀點而言,以鉻、鎳、鈦、鋁、鋅、金、鈀、銀或銅的單金屬層、或鎳‧鉻合金、銅‧鎳合金、銅‧鈦合金的合金層為較佳,以鉻、鎳、鈦、鋁、鋅、金、鈀、銀或銅的單金屬層、或鎳‧鉻合金的合金層為又較佳,以銅的單金屬層為更佳。
導體層可以是單層構造,亦可以是層合2層以上由不同種類的金屬或合金所成之單金屬層或合金層之多層構造。若導體層為多層構造時,與絕緣層相接的層係以鉻、鋅或鈦的單金屬層、或鎳‧鉻合金的合金層為較佳。
導體層的厚度係依所期望的印刷配線板之設計而定,但一般為3μm~35μm,較佳為5μm~30μm。
一實施形態中,導體層係可藉由鍍敷來形成。可藉由例如半加成法、全加成法等的以往周知的技術鍍敷在絕緣層之表面,從而形成具有所期望的配線圖型之導體層。以下,表示藉由半加成法來形成導體層之例。
首先,在絕緣層之表面上,藉由無電解鍍敷來形成鍍敷種晶層。接下來,在所形成的鍍敷種晶層上,對應所期望的配線圖型,形成使鍍敷種晶層的一部分露出
之遮罩圖型。在露出的鍍敷種晶層上,藉由電解鍍敷來形成金屬層後,將遮罩圖型除去。之後,可藉由蝕刻等除去不需要的鍍敷種晶層,從而形成具有所期望的配線圖型之導體層。
本發明之樹脂薄片係因可產生零件埋置性亦為良好的絕緣層,故可適合使用於若印刷配線板為零件內附電路板之情形時。零件內附電路板係可藉由周知的製造方法來製作。
使用本發明之樹脂薄片來製造之印刷配線板,係可以是具備有本發明之樹脂薄片之樹脂組成物層之硬化物之絕緣層、與埋置在絕緣層之埋置型配線層之樣態。
使用本發明之樹脂薄片來製造之印刷配線板,即便是第1及第2導體層之間的絕緣層之厚度為6μm以下,亦可展現出絕緣可靠性為優異之特性。以130℃下、85RH%、外加3.3V環境下,經過100小時後之絕緣電阻值之上限,較佳為1012Ω以下,又較佳為1011Ω以下,更佳為1010Ω以下。下限並無特別限定,較佳為106Ω以上,又較佳為107Ω以上。絕緣電阻值之測定,係可根據後述之<絕緣可靠性之評估、導體層之間的絕緣層之厚度之測定>所記載之方法來進行測定。
[半導體裝置]
本發明之半導體裝置係包含本發明之印刷配線板。本
發明之半導體裝置係可使用本發明之印刷配線板來製造。
作為半導體裝置,可舉出提供於電氣製品(例如電腦、行動電話、數位相機及電視等)及交通工具(例如摩托車、汽車、火車、船舶及飛機等)等之各種半導體裝置。
本發明之半導體裝置係可藉由在印刷配線板的導通部位安裝零件(半導體晶片)來製造。所謂的「導通部位」,係指「印刷配線板中之傳遞電訊號的部位」,且該位置係可為表面,亦可為被埋置的部位中任何皆可。
又,半導體晶片只要是將半導體作為材料之電路元件即可,並無特別限定。
製造本發明之半導體裝置時之半導體晶片之安裝方法,只要是半導體晶片能有效地發揮功能即可,並無特別限定,具體而言可舉出導線接合安裝方法、倒裝晶片安裝方法、藉由無凸塊增層(BBUL)之安裝方法、藉由異向性導電薄片(ACF)之安裝方法、藉由非導電性薄片(NCF)之安裝方法等。於此,所謂的「藉由無凸塊增層(BBUL)之安裝方法」,係指「將半導體晶片直接埋置在印刷配線板的凹部,並使半導體晶片與印刷配線板上的配線連接之安裝方法」。
[實施例]
以下藉由實施例具體的說明本發明,但本發明並非被限定於該等之實施例。尚,以下之記載中,
「份」及「%」只要無特別說明,分別為「質量份」及「質量%」之意。
[無機填充材之物性值之測定方法]
首先,對於實施例及比較例中使用的無機填充材之物性值之測定方法來進行說明。
<平均粒徑之測定>
將無機填充材100mg、分散劑(Sannopco(股)製「SN9228」)0.1g、甲基乙基酮10g秤取至管形瓶中,藉以超音波進行分散20分鐘。使用雷射繞射式粒度分布測定裝置((股)島津製作所製「SALD-2200」),以分批槽方式來測定粒度分布,並算出藉由均粒徑之平均粒徑。
<比表面積之測定>
使用BET全自動比表面積測定裝置(Mountech(股)製「Macsorb HM-1210」),測定無機填充材之比表面積。
<真密度之測定>
使用超微比重計(Quantachrome Instruments Japan製「MUPY-21T」),測定無機填充材之真密度。
<碳量之測定>
無機填充材之每單位表面積的碳量,係根據以下之程
序來進行測定。在調製例所調製的無機填充材中,加入作為溶劑之充分量的MEK,並以25℃下進行超音波洗淨5分鐘。接下來,除去上清液,並使固形分乾燥。對於所得到之固體,使用碳分析計((股)堀場製作所製「EMIA-320V」)測定碳量。基於碳量的測定值、與使用的無機填充材的質量及比表面積,來算出無機填充材的每單位表面積的碳量。
[樹脂薄片之製作]
依據以下之程序,來調製樹脂薄片之製作中使用之樹脂組成物(亦稱為「樹脂清漆」),並製作實施例及比較例之樹脂薄片。
(樹脂組成物1之調製)
對於雙酚A型環氧樹脂(新日鐵住金化學(股)製「YD-8125G」、環氧當量約174)4份、聯二甲酚型環氧樹脂(三菱化學(股)製「YX4000HK」、環氧當量約185)6份、雙酚AF型環氧樹脂(三菱化學(股)製「YL7760」、環氧當量約238)6份、聯苯型環氧樹脂(日本化藥(股)製「NC3000L」、環氧當量約272)18份、苯氧基樹脂(三菱化學(股)製「YX7553BH30」,固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)10份、及溶劑石油腦10份及環己酮10份的混合溶劑,一邊攪拌並一邊使其加熱溶解。冷卻至室溫後,於此中混合含有三嗪骨架之苯酚酚醛
清漆系硬化劑(DIC(股)製「LA7052」、羥基當量約120、固形分60%的MEK溶液)10份、萘酚系硬化劑(新日鐵住金化學(股)製「SN-495V」、羥基當量231、固形分60%的MEK溶液)12份、碳二亞胺樹脂(日清紡Chemical(股)製「V-03」、碳二亞胺當量216、不揮發成分50質量%的甲苯溶液)10份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)1份、使橡膠粒子(Aica工業(股)製、AC-3401N)2份在溶劑石油腦10份中在室溫下膨潤12小時者、經胺基矽烷系偶合劑(信越化學工業(股)製「KBM573」)表面處理的球狀矽石(新日鐵住金MATERIALS(股)製「SPH516-05」、平均粒徑0.29μm、比表面積16.3m2/g、真密度2.25g/cm3、比表面積與真密度的積36.7(m2/g‧g/cm3)、每單位表面積的碳量0.43mg/m2)110份,利用高速旋轉混合器均勻地分散後,並以濾筒(ROKITECHNO製「SHP020」)進行過濾來調製樹脂組成物1。
(樹脂組成物2之調製)
將萘型環氧樹脂(DIC(股)製「HP4032SS」、環氧當量約144)4份、伸萘基醚型環氧樹脂(DIC(股)製「EXA-7311-G4」、環氧當量約213)8份、萘型環氧樹脂(新日鐵住金化學(股)製「ESN475V」、環氧當量約330)15份、及苯氧基樹脂(三菱化學(股)製「YX7553BH30」、固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)6份,在溶
劑石油腦15份及環己酮10份的混合溶劑中一邊攪拌,一邊使其加熱溶解。冷卻至室溫後,於此中混合雙酚A二氰酸酯的預聚物(Lonza Japan(股)製「BA230S75」、氰酸酯當量約232、不揮發分75質量%的MEK溶液)18份、多官能氰酸酯樹脂(Lonza Japan(股)製「ULL-950S」、氰酸酯當量約230、不揮發分75質量%的MEK溶液)10份、活性酯系硬化劑(DIC(股)製「HPC-8000-65T」、活性基當量約225、不揮發成分65質量%的甲苯溶液)6份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)0.4份、硬化促進劑(東京化成(股)製、乙醯丙酮酸鈷(III)(Co(III)Ac)、固形分1質量%的MEK溶液)3份、經胺基矽烷系偶合劑(信越化學工業(股)製「KBM573」)表面處理的球狀矽石(新日鐵住金MATERIALS(股)製「SPH516-05」、平均粒徑0.29μm、比表面積16.3m2/g、真密度2.25g/cm3、比表面積與真密度的積36.7(m2/g‧g/cm3)、每單位表面積的碳量0.43mg/m2)90份,利用高速旋轉混合器均勻地分散後,並以濾筒(ROKITECHNO製「SHP020」)進行過濾來調製樹脂組成物2。
(樹脂組成物3之調製)
將縮水甘油胺型環氧樹脂(三菱化學(股)製「630LSD」、環氧當量約95)4份、聯二甲酚型環氧樹脂(三菱化學(股)製「YX4000HK」、環氧當量約185)5份、伸萘基醚型環氧樹脂(DIC(股)製「EXA-7311-G4」、環氧
當量約213)5份、聯苯型環氧樹脂(日本化藥(股)製「NC3000L」、環氧當量約272)15份、及苯氧基樹脂(三菱化學(股)製「YX7553BH30」、固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)10份,在溶劑石油腦15份及環己酮10份的混合溶劑中一邊攪拌,一邊使其加熱溶解。冷卻至室溫後,於此中混合含有三嗪骨架之甲酚酚醛清漆系硬化劑(DIC(股)製「LA3018-50P」、羥基當量約151、固形分50%的2-甲氧基丙醇溶液)5份、活性酯系硬化劑(DIC(股)製「HPC-8000-65T」、活性基當量約225、不揮發成分65質量%的甲苯溶液)15份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)1.5份、耐燃劑(三光(股)製「HCA-HQ」、10-(2,5-羥基苯基)-10-氫-9-氧雜-10-磷雜菲-10-氧化物、平均粒徑1.2μm)2份、經胺基矽烷系偶合劑(信越化學工業(股)製「KBM573」)表面處理的球狀矽石(新日鐵住金MATERIALS(股)製「SPH516-05」、平均粒徑0.29μm、比表面積16.3m2/g、真密度2.25g/cm3、比表面積與真密度的積36.7(m2/g‧g/cm3)、每單位表面積的碳量0.43mg/m2)110份,利用高速旋轉混合器均勻地分散後,並以濾筒(ROKITECHNO製「SHP020」)進行過濾來調製樹脂組成物3。
(樹脂組成物4之調製)
對於雙酚A型環氧樹脂(三菱化學(股)製「828EL」、
環氧當量約186)8份、雙酚AF型環氧樹脂(三菱化學(股)製「YL7760」、環氧當量約238)6份、聯苯型環氧樹脂(日本化藥(股)製「NC3000L」、環氧當量約272)18份、苯氧基樹脂(三菱化學(股)製「YX7553BH30」、固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)10份、及溶劑石油腦5份及環己酮10份的混合溶劑,一邊攪拌並一邊使其加熱溶解。冷卻至室溫後,於此中混合含有三嗪骨架之苯酚酚醛清漆系硬化劑(DIC(股)製「LA7052」、羥基當量約120、固形分60%的MEK溶液)10份、萘酚系硬化劑(新日鐵住金化學(股)製「SN-495V」、羥基當量231、固形分60%的MEK溶液)12份、嵌段型異氰酸酯樹脂(DIC(股)製「BURNOCK D-500」、不揮發成分65質量%的乙酸乙酯溶液)5份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)1份、使橡膠粒子(Aica工業(股)製、AC-3355)6份在溶劑石油腦15份中在室溫下膨潤12小時者、經胺基矽烷系偶合劑(信越化學工業(股)製「KBM573」)表面處理的球狀矽石(Admatechs(股)製「Admafine SO-C1」、平均粒徑0.63μm、比表面積11.2m2/g、真密度2.25g/cm3、比表面積與真密度的積25.2(m2/g‧g/cm3)、每單位表面積的碳量0.35mg/m2)110份,利用高速旋轉混合器均勻地分散後,並以濾筒(ROKITECHNO製「SHP030」)進行過濾來調製樹脂組成物4。
(樹脂組成物5之調製)
將萘型環氧樹脂(DIC(股)製「HP4032SS」、環氧當量約144)4份、雙酚A型環氧樹脂(三菱化學(股)製「828EL」、環氧當量約186)8份、萘型環氧樹脂(新日鐵住金化學(股)製「ESN475V」、環氧當量約330)15份、及苯氧基樹脂(三菱化學(股)製「YX7553BH30」、固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)6份,在溶劑石油腦10份及環己酮10份的混合溶劑中一邊攪拌,一邊使其加熱溶解。冷卻至室溫後,於此中混合雙酚A二氰酸酯的預聚物(Lonza Japan(股)製「BA230S75」、氰酸酯當量約232、不揮發分75質量%的MEK溶液)18份、多官能氰酸酯樹脂(Lonza Japan(股)製「ULL-950S」、氰酸酯當量約230、不揮發分75質量%的MEK溶液)10份、嵌段型異氰酸酯樹脂(DIC(股)製「BURNOCK D-500」、不揮發成分65質量%的乙酸乙酯溶液)6份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)0.4份、硬化促進劑(東京化成(股)製、乙醯丙酮酸鈷(III)(Co(III)Ac)、固形分1質量%的MEK溶液)3份、經環氧基矽烷系偶合劑(信越化學工業(股)製「KBM403」)表面處理的球狀矽石(Admatechs(股)製「Admafine SO-C1」、平均粒徑0.63μm、比表面積11.2m2/g、真密度2.25g/cm3、比表面積與真密度的積25.2(m2/g‧g/cm3)、每單位表面積的碳量0.25mg/m2)90份,利用高速旋轉混合器均勻地分散後,並以濾筒(ROKITECHNO製
「SHP030」)進行過濾來調製樹脂組成物5。
(樹脂組成物6之調製)
將雙酚F型環氧樹脂(三菱化學(股)製「806L」、環氧當量約185)4份、聯二甲酚型環氧樹脂(三菱化學(股)製「YX4000HK」、環氧當量約185)5份、伸萘基醚型環氧樹脂(DIC(股)製「EXA-7311-G4」、環氧當量約213)5份、聯苯型環氧樹脂(日本化藥(股)製「NC3000L」、環氧當量約272)15份、及苯氧基樹脂(三菱化學(股)製「YX7553BH30」、固形分30質量%的環己酮:甲基乙基酮(MEK)的1:1溶液)10份、耐燃劑(大八化學工業(股)製「PX-200」)4份,在溶劑石油腦15份及環己酮10份的混合溶劑中一邊攪拌,一邊使其加熱溶解。冷卻至室溫後,於此中混合含有三嗪骨架之甲酚酚醛清漆系硬化劑(DIC(股)製「LA3018-50P」、羥基當量約151、固形分50%的2-甲氧基丙醇溶液)5份、活性酯系硬化劑(DIC(股)製「HPC-8000-65T」、活性基當量約225、不揮發成分65質量%的甲苯溶液)15份、胺系硬化促進劑(4-二甲基胺吡啶(DMAP)、固形分5質量%的MEK溶液)1.5份、經胺基矽烷系偶合劑(信越化學工業(股)製「KBM573」)表面處理的球狀矽石(Admatechs(股)製「Admafine SO-C1」、平均粒徑0.63μm、比表面積11.2m2/g、真密度2.25g/cm3、比表面積與真密度的積25.2(m2/g‧g/cm3)、每單位表面積的碳量0.35mg/m2)110份,利用高速旋轉混合器均勻地分散
後,並以濾筒(ROKITECHNO製「SHP030」)進行過濾來調製樹脂組成物6。
將樹脂組成物1~6中使用的成分與其調配量(不揮發分之質量份)表示於下述表中。
(實施例1-1~1-3及實施例2-1~2-3之樹脂薄片、以及、比較例1-1~1-3及比較例2-1~2-3之樹脂薄片之製作)
作為支撐體,準備利用醇酸樹脂系脫模劑(Lintec(股)製「AL-5」)進行脫模處理之PET薄片(Toray(股)製「Lumirror R80」、厚度38μm、軟化點130℃、「脫模PET」)。
將各樹脂組成物藉由模塗布機,以乾燥後之樹脂組成物層之厚度成為13μm之方式,在脫模PET上均勻地塗布,並藉由從70℃至95℃下乾燥2分鐘,從而在脫模PET上來形成樹脂組成物層。接下來,在未與樹脂組成物層之支撐體接合的面上,以與樹脂組成物層接合之方式,來層合作為保護薄片之聚丙烯薄片(王子F-tex股)製「ALPHAN MA-411」、厚度15μm)的粗面。據此,可得到由支撐體、樹脂組成物層、及保護薄片之順序所成之樹脂薄片。
另外,除了將各樹脂組成物藉由模塗布機,以乾燥後之樹脂組成物層之厚度成為10μm之方式,在脫模PET上均勻地塗布以外,與上述相同之方式,來製作由支撐體、厚度為10μm之樹脂組成物層、及保護薄片之順序所成之樹脂薄片。
[評估試驗]
<最低熔融黏度之測定>
對於實施例1-1~1-3及實施例2-1~2-3之樹脂薄片、
以及比較例1-1~1-3及比較例2-1~2-3之樹脂薄片,依據下述之方法來測定最低熔融黏度。
使用樹脂組成物層之厚度為13μm之樹脂薄片,僅將樹脂組成物層從脫模PET(支撐體)剝離,藉由使用模具進行壓縮,從而製作測定用顆粒(直徑18mm、1.2~1.3g)。
利用動態黏彈性測定裝置(UBM(股)製「Rheosol-G3000」),對於樣品樹脂組成物層1g,使用直徑18mm的平行板,藉以昇溫速度5℃/分下從開始溫度60℃至200℃進行昇溫,並藉以測定溫度間隔2.5℃、振動數1Hz、應變1deg之測定條件下測定動態黏彈性率來算出最低熔融黏度(poise),並表示於表2及表3中。
<硬化物之玻璃移轉溫度之測定(實施例1-1~1-3及比較例1-1~1-3)>
依據以下之方法來測定實施例1-1~1-3及比較例1-1~1-3之樹脂薄片之樹脂組成物層之硬化物之玻璃移轉溫度。脫模PET薄片(Lintec(股)製「501010」、厚度38μm、240mm見方)的未處理面,以與玻璃布基材環氧樹脂雙面銅箔層合板(松下電工(股)製「R5715ES」、厚度0.7mm、255mm見方)相接之方式,來設置在玻璃布基材環氧樹脂雙面銅箔層合板上,並用聚醯亞胺接著膠帶(寬10mm)固定該脫模PET薄片的四邊。
使用分批式真空加壓貼合機(Nikko-materials
(股)製2階段增層貼合機、CVP700),以樹脂組成物層與脫模PET薄片(Lintec(股)製「501010」)的脫模面相接之方式,將實施例及比較例所製作之樹脂組成物層之厚度為13μm的各樹脂薄片(200mm見方),在中央進行層合處理。層合處理係藉由減壓30秒鐘並將氣壓設為13hPa以下後,以100℃、壓力0.74MPa下使其壓黏30秒鐘來進行實施。
接下來,以100℃的溫度條件下,投入100℃的烘箱後30分鐘,接下來,以175℃的溫度條件下,轉移至175℃的烘箱後30分鐘,並使其熱硬化。之後,將基板在室溫環境下取出,並從樹脂薄片剝離脫模PET(支撐體)後,進而以投入至190℃的烘箱後90分鐘之硬化條件下使其熱硬化。
熱硬化後剝下聚醯亞胺接著膠帶,從玻璃布基材環氧樹脂雙面銅箔層合板上取下硬化物。進而剝離層合著樹脂組成物層的脫模PET薄片(Lintec(股)製「501010」),從而可得到薄片狀的硬化物。將所得到之硬化物稱為「評估用硬化物」。
將上述「評估用硬化物」裁切成寬約7mm、長度約40mm的試片,並使用動態機械分析裝置DMS-6100(Seiko Instruments(股)製),藉以拉伸模式來進行動態機械分析(DMA)。相關之測定係藉以頻率1Hz、2℃/分的昇溫在25℃~240℃的範圍內來進行。將由測定所得到之儲能彈性率(E')與損失彈性率(E”)之比所求得之損失正切
(tan δ)的最大值四捨五入小數點第一位的值設為玻璃移轉溫度(℃),並表示於表2中。
<硬化物之萃取水導電率之測定(實施例1-1~1-3及比較例1-1~1-3)>
將依<硬化物之玻璃移轉溫度之測定>之一項中所製作的「評估用硬化物」,使用粉碎機(大阪chemical(股)製PM-2005m)來進行粉碎,並進行粉碎物的篩分,將通過150μm、不通過75μm的分離2.0g,與超純水40g一起放入耐壓容器並密封。尚,將在相同的容器中放入超純水50g並密封者設為空白試樣(blank)。萃取條件係設以120℃下20小時或160℃下20小時。萃取後,藉以冰水快速地冷卻容器,並用膜片過濾器(Millipore製MILLEX-GV0.22μm)來過濾萃取懸濁水。與空白試樣一起來測定過濾後的各萃取水之導電率,由以下之計算式來算出萃取水導電率,並表示於表2中。
萃取水導電率(μS/cm)=萃取水之導電率-空白試樣之導電率
<硬化物之拉伸破壞強度之測定(實施例2-1~2-3及比較例2-1~2-3)>
對於實施例2-1~2-3之樹脂薄片及比較例2-1~2-3之樹脂薄片,依據以下之方法來測定硬化物之拉伸破壞強度。
以脫模PET薄片(Lintec(股)製「501010」、厚度38μm、240mm見方)之未處理面與玻璃布基材環氧樹脂雙面銅箔層合板(松下電工(股)製「R5715ES」、厚度0.7mm、255mm見方)相接之方式,來設置在玻璃布基材環氧樹脂雙面銅箔層合板上,並用聚醯亞胺接著膠帶(寬10mm)固定該脫模PET薄片的四邊。
使用分批式真空加壓貼合機(Nikko-materials(股)製2階段增層貼合機、CVP700),以樹脂組成物層與脫模PET薄片(Lintec(股)製「501010」)的脫模面相接之方式,將實施例及比較例所製作之樹脂組成物層之厚度為10μm的各樹脂薄片(200mm見方),在中央進行層合處理。層合處理係藉由減壓30秒鐘並將氣壓設為13hPa以下後,以100℃、壓力0.74MPa下使其壓黏30秒鐘來進行實施。
接下來,以100℃的溫度條件下,投入100℃的烘箱後30分鐘,接下來,以175℃的溫度條件下,轉移至175℃的烘箱後30分鐘,並使其熱硬化。之後,將基板在室溫環境下取出,並從樹脂薄片剝離脫模PET(支撐體)後,進而以投入至190℃的烘箱後90分鐘之硬化條件下使其熱硬化。
熱硬化後,對於進行HAST試驗(Highly Accelerated temperature and humidity Stress Test)者,在此狀態下使用高度加速壽命試驗裝置(ETAC製「PM422」),以130℃、85%的相對濕度之條件下使其經
過100小時。之後剝下聚醯亞胺接著膠帶,從玻璃布基材環氧樹脂雙面銅箔層合板上取下硬化物,進而剝離層合著樹脂組成物層之脫模PET薄片(Lintec(股)製「501010」),從而可得到HAST試驗後之厚度為10μm的薄片狀硬化物。對於未進行HAST試驗者,熱硬化後剝下聚醯亞胺接著膠帶,從玻璃布基材環氧樹脂雙面銅箔層合板上取下硬化物,進而剝離層合著樹脂組成物層之脫模PET薄片,從而可得到厚度為10μm的薄片狀硬化物。以如此般之方式所得到之硬化物中,將在硬化後未進行HAST試驗者稱為「評估用硬化物A」,將在硬化後進行HAST試驗者稱為「評估用硬化物B」。
將「評估用硬化物A」及「評估用硬化物B」分別裁切成啞鈴狀,從而可得到試片。將該試片依據JIS K7127,使用Orientec公司製、拉伸試驗機RTC-1250A來進行拉伸強度測定,可求得在23℃中之拉伸破壞強度(MPa)。測定係對於5樣品來進行,並將前3位測量值之平均值表示於表3中。表3中,所謂的「硬化物之拉伸破壞強度A」係指評估用硬化物A之拉伸破壞強度(MPa),所謂的「HAST試驗後之硬化物之拉伸破壞強度B」係指評估用硬化物B之拉伸破壞強度(MPa),所謂的「B/A」係指「拉伸破壞強度B/拉伸破壞強度A」。
<絕緣可靠性之評估、導體層之間的絕緣層之厚度之測定>
對於實施例1-1~1-3及實施例2-1~2-3之樹脂薄片、以及比較例1-1~1-3及比較例2-1~2-3之樹脂薄片,依據下述之方法來進行絕緣可靠性之評估試驗,同時測定導體層之間的絕緣層之厚度。
(評估用基板之調製)
(1)內層電路基板之基底處理
作為內層電路基板,準備在雙面具有以1mm見方格子的配線圖型(殘銅率為59%)所形成的電路導體(銅)之玻璃布基材環氧樹脂雙面銅箔層合板(銅箔之厚度18μm、基板之厚度0.3mm、panasonic(股)製「R1515F」)。將該內層電路基板的雙面,藉以MEC(股)製「CZ8201」來進行銅表面之粗化處理(銅蝕刻量0.5μm)。
(2)樹脂薄片之層合
使用分批式真空加壓貼合機(Nikko-materials(股)製、2階段增層貼合機、CVP700),以樹脂組成物層與內層電路基板相接之方式,將實施例及比較例所製作之各樹脂薄片(樹脂組成物層之厚度為13μm者)層合在內層電路基板的雙面。層合係藉由減壓30秒鐘並將氣壓設為13hPa以下,以130℃、壓力0.74MPa下使其壓黏45秒鐘來進行實施。接下來,以120℃、壓力0.5MPa下來進行熱壓製75秒鐘。
(3)樹脂組成物層之熱硬化
將層合著樹脂薄片之內層電路基板,以100℃的溫度條件下,投入至100℃的烘箱後30分鐘,接下來,以175℃的溫度條件下,轉移至175℃的烘箱後30分鐘,進行熱硬化從而形成絕緣層。
(4)通孔洞之形成
從絕緣層及支撐體之上方起,使用三菱電機(股)製CO2雷射加工機「605GTWIII(-P)」,由支撐體的上方來照射雷射,並在格子圖型的導體上之絕緣層,形成頂端口徑(70μm)的通孔洞。雷射的照射條件係以遮罩徑為2.5mm,脈衝寬為16μs,能量為0.39mJ/發射,發射數為2,脈衝間歇模式(10kHz)下來進行。
(5)進行粗化處理之步驟
從設置有通孔洞的電路基板來剝離支撐體,並進行除膠渣處理。尚,作為除膠渣處理係實施下述之濕式除膠渣處理。
濕式除膠渣處理:
在膨潤液(Atotech Japan(股)製「Swelling Dip Securigant P」、二乙二醇單丁基醚及氫氧化鈉的水溶液)中以60℃下浸漬5分鐘,接下來,在氧化劑溶液(Atotech Japan(股)製「concentrate Compact CP」、過錳酸鉀濃度
約6%、氫氧化鈉濃度約4%的水溶液)中以80℃下浸漬10分鐘,最後在中和液(Atotech Japan(股)製「Reduction solution Securiganth P」、硫酸水溶液)以40℃下浸漬5分鐘後,以80℃下乾燥15分鐘。
(6)形成導體層之步驟
(6-1)無電解鍍敷步驟
為了在上述電路基板的表面上形成導體層,進行包含下述1~6之步驟之鍍敷步驟(使用Atotech Japan(股)製的藥液之銅鍍敷步驟),從而形成導體層。
1.鹼清潔(設置有通孔洞之絕緣層的表面之洗淨與電荷調整)
商品名:使用Cleaning Cleaner Securiganth 902(商品名),以60℃下洗淨5分鐘。
2.軟蝕刻(通孔洞內之洗淨)
使用硫酸酸性過氧二硫酸鈉水溶液,以30℃下處理1分鐘。
3.預浸漬(用於賦予Pd之絕緣層表面之電荷之調整)
使用Pre.Dip Neoganth B(商品名),以室溫下處理1分鐘。
4.活化劑賦予(對於絕緣層的表面之Pd的賦予)
使用Activator Neoganth 834(商品名),以35℃下處理5分鐘。
5.還原(還原賦予於絕緣層的Pd)
使用Reducer Neoganth WA(商品名)與Reducer Acceralator 810 mod.(商品名)的混合液,以30℃下處理5分鐘。
6.無電解銅鍍敷步驟(將Cu在絕緣層的表面(Pd表面)上析出)
使用Basic Solution Printganth MSK-DK(商品名)、Copper solution rintganth MSK(商品名)、與Stabilizer Printganth MSK-DK(商品名)、及Reducer Cu(商品名)的混合液,以35℃下處理20分鐘。所形成的無電解銅鍍敷層之厚度為0.8μm。
(6-2)電解鍍敷步驟
接下來,使用Atotech Japan(股)製的藥液,以在通孔洞內填充銅之條件下來進行電解銅鍍敷步驟。之後,作為用於藉由蝕刻之圖型化之阻劑圖型,使用與通孔洞所導通的直徑1mm的焊盤圖型(land pattern),及未與下層導體連接的直徑10mm的圓形導體圖型,在絕緣層的表面上以10μm之厚度來形成具有焊盤及導體圖型之導體層。接下來,將退火處理以190℃下進行90分鐘,並將所得到之基板作為評估用基板A。
(7)導體層之間的絕緣層之厚度之測定
將評估用基板A使用FIB-SEM複合裝置
(SIINanoTechnology(股)製「SMI3050SE」)來進行截面觀察。詳細而言係藉由FIB(聚焦離子束)削出與導體層的表面呈垂直方向之截面,由截面SEM圖像來測定導體層之間的絕緣層厚度。對於每個樣品觀察隨機所選出的5部位的截面SEM圖像,並將該平均值作為導體層之間的絕緣層之厚度表示於表2及表3中。
(8)絕緣層之絕緣可靠性之評估
將上述中所得到之評估用基板A的直徑10mm之圓形導體側作為正(+)電極,將與直徑1mm的焊盤連接的內層電路基板之格子導體(銅)側作為負(-)電極,藉由Electro Chemical Migration Tester(J-RAS(股)製「ECM-100」),測定使用高度加速壽命試驗裝置(ETAC製「PM422」)以130℃、85%相對濕度、外加3.3V直流電壓之條件下經過200小時之際的絕緣電阻值(n=6)。全部6個試片中其絕緣電阻值為107Ω以上之情形時設為「○」,只要1個未滿107Ω之情形時設為「×」,將評估結果表示於表2及表3中。表2及表3所記載之絕緣電阻值,係6個試片之絕緣電阻值之中的最低值。
Claims (14)
- 一種樹脂薄片,其係包含支撐體、與接合在該支撐體上的樹脂組成物層,該樹脂組成物層係由含有(A)環氧樹脂及(B)硬化劑,且[環氧樹脂的環氧基的合計數]:[硬化劑的反應基的合計數]之比率計為1:0.01~1:2的樹脂組成物所成,該樹脂組成物層之硬化物在120℃下20小時的萃取水導電率A為50μS/cm以下,且該樹脂組成物層之硬化物在160℃下20小時的萃取水導電率B為200μS/cm以下。
- 如請求項1之樹脂薄片,其中,樹脂組成物層之硬化物的玻璃移轉溫度為160℃以上。
- 一種樹脂薄片,其係包含支撐體、與接合在該支撐體上的樹脂組成物層,該樹脂組成物層係由含有(A)環氧樹脂及(B)硬化劑,且[環氧樹脂的環氧基的合計數]:[硬化劑的反應基的合計數]之比率計為1:0.01~1:2的樹脂組成物所成,該樹脂組成物層之硬化物且厚度為10μm之硬化物之HAST(高溫高濕試驗)後之拉伸破壞強度B,對該樹脂組成物層之硬化物且厚度為10μm之硬化物之拉伸破壞強度A之比(B/A)為0.65以上1以下。
- 如請求項3之樹脂薄片,其中,前述拉伸破壞強度B為50MPa以上。
- 如請求項1或3之樹脂薄片,其中,樹脂組成物層 之厚度為15μm以下。
- 如請求項1或3之樹脂薄片,其中,樹脂組成物層之最低熔融黏度為1000poise以上。
- 如請求項1或3之樹脂薄片,其中,樹脂組成物層含有環氧樹脂及硬化劑。
- 如請求項1或3之樹脂薄片,其中,若樹脂組成物層含有無機填充材、且將樹脂組成物層中之不揮發成分設為100質量%時,該無機填充材的含有量為50質量%以上。
- 如請求項8之樹脂薄片,其中,該無機填充材之平均粒徑為0.05μm~0.35μm。
- 如請求項8之樹脂薄片,其中,該無機填充材之比表面積[m2/g]與真密度[g/cm3]之乘積為0.1~77。
- 如請求項1或3之樹脂薄片,其係印刷配線板之絕緣層形成用。
- 如請求項1或3之樹脂薄片,其係包含第1導體層、第2導體層、與絕緣第1導體層和第2導體層的絕緣層、且第1導體層和第2導體層之間的絕緣層之厚度為6μm以下的印刷配線板之該絕緣層形成用。
- 一種印刷配線板,其係包含第1導體層、第2導體層、與絕緣第1導體層和第2導體層的絕緣層、且第1導體層和第2導體層之間的絕緣層之厚度為6μm以下,該絕緣層係請求項1或3之樹脂薄片之樹脂組成物層之硬化物。
- 一種半導體裝置,其係包含請求項13之印刷配線板。
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- 2017-03-27 KR KR1020170038741A patent/KR102398708B1/ko active IP Right Grant
- 2017-03-29 US US15/472,684 patent/US10257928B2/en active Active
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US20190200455A1 (en) | 2019-06-27 |
JP6672953B2 (ja) | 2020-03-25 |
JP2017177461A (ja) | 2017-10-05 |
TW201806740A (zh) | 2018-03-01 |
KR20170113296A (ko) | 2017-10-12 |
US20170290149A1 (en) | 2017-10-05 |
CN107236253A (zh) | 2017-10-10 |
KR102398708B1 (ko) | 2022-05-17 |
US10257928B2 (en) | 2019-04-09 |
US10512161B2 (en) | 2019-12-17 |
CN107236253B (zh) | 2023-05-30 |
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