TWI760301B - 樹脂組成物、預浸體、覆金屬箔疊層板、樹脂片及印刷電路板 - Google Patents
樹脂組成物、預浸體、覆金屬箔疊層板、樹脂片及印刷電路板 Download PDFInfo
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- TWI760301B TWI760301B TW105112537A TW105112537A TWI760301B TW I760301 B TWI760301 B TW I760301B TW 105112537 A TW105112537 A TW 105112537A TW 105112537 A TW105112537 A TW 105112537A TW I760301 B TWI760301 B TW I760301B
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- -1 prepreg Substances 0.000 title claims description 81
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- 229920000647 polyepoxide Polymers 0.000 claims abstract description 71
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- 239000011888 foil Substances 0.000 claims description 12
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 9
- 125000005605 benzo group Chemical group 0.000 claims description 8
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- 239000004020 conductor Substances 0.000 claims description 5
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- 125000005439 maleimidyl group Chemical class C1(C=CC(N1*)=O)=O 0.000 claims description 2
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- 229920003986 novolac Polymers 0.000 description 24
- 238000000034 method Methods 0.000 description 23
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- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 13
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 4
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- 239000004408 titanium dioxide Substances 0.000 description 1
- 125000004360 trifluorophenyl group Chemical group 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 description 1
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 1
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Abstract
本發明提供一種樹脂組成物,含有氰酸酯化合物(A)及下列通式(1)表示之環氧樹脂(B); 【化1】
Description
本發明係關於樹脂組成物、預浸體、覆金屬箔疊層板、樹脂片及印刷電路板。
近年來,廣泛使用於電子設備或通訊器材、個人電腦等之半導體更加速地高積體化及小型化。伴隨於此,對於印刷電路板使用之半導體封裝用疊層板之各種特性之要求變得越來越嚴格。就要求的特性而言,可舉例如低吸水性、吸濕耐熱性、阻燃性、低介電係數、低介電正切、低熱膨脹率、耐熱性、耐藥品性、高鍍敷剝離強度等特性。然而,到目前為止並非一定可滿足此等要求特性。
以往,就耐熱性或電特性優良之印刷電路板用樹脂而言,已知有氰酸酯化合物,其中將氰酸酯化合物與環氧樹脂等併用的樹脂組成物近年來廣泛地使用於半導體塑膠封裝體用等之高性能之印刷電路板用材料等。此外,由於多層印刷電路板之小型化、高密度化,多層印刷電路板有使增建層多層化、佈線之微細化及高密度化之需求。 [先前技術文獻] [專利文獻]
專利文獻1:國際公開第2013/065694號小冊 專利文獻2:國際公開第2014/203866號小冊 專利文獻3:日本專利第5413522號公報
[發明所欲解決之課題] 此處,有人提出密合性、低吸水性、吸濕耐熱性、絕緣可靠性等特性優良之由氰酸酯化合物及環氧樹脂構成之樹脂組成物(例如,參照專利文獻1、2),但針對鍍敷剝離強度仍不夠充分,故有更提高鍍敷剝離強度之需求。
此外,就提高銅箔之剝離強度及鍍敷剝離強度之方法而言,有人提出將填充材進行表面處理之方法(參照專利文獻3),但針對鍍敷剝離強度仍不夠充分,故有更提高鍍敷剝離強度之需求。
因此,本發明為以上述習知技術之問題為鑑所產生者,目的為提供可獲得耐熱性優良且鍍敷密合性也優良之硬化物而可達成鍍敷剝離強度優良之印刷電路板的樹脂組成物。 [解決課題之手段]
本案發明者們針對上述課題深入研究之結果發現,藉由使用含有氰酸酯化合物(A)及具有指定之結構之環氧樹脂(B)的樹脂組成物,可獲得耐熱性優良且鍍敷密合性也優良之硬化物,而可獲得具有高鍍敷剝離強度之印刷電路板,而完成了本發明。也就是說,本發明如同下述。
[1] 一種樹脂組成物,含有氰酸酯化合物(A)及下列通式(1)表示之環氧樹脂(B); 【化1】式中,m及n各自獨立地表示1以上之整數;該通式(1)表示之環氧樹脂(B)也可為m及n各自獨立地代表不同整數之化合物之混合物。 [2] 如[1]之樹脂組成物,其中,該通式(1)表示之環氧樹脂(B)之含量相對於該樹脂組成物中之樹脂固體成分之總量(100質量份)為1~90質量份。 [3] 如[1]或[2]之樹脂組成物,更含有填充材(C)。 [4] 如[1]~[3]任一項之樹脂組成物,更含有選自於由該通式(1)表示之環氧樹脂(B)以外之環氧樹脂、馬來醯亞胺化合物、苯酚樹脂、氧雜環丁烷樹脂、苯并
化合物、及具有可聚合之不飽和基之化合物構成之群組中之1種或2種以上。 [5] 如[3]或[4]之樹脂組成物,其中,該填充材(C)之含量相對於該樹脂組成物中之樹脂固體成分之總量(100質量份)為50~1600質量份。 [6] 一種預浸體,具有:基材;及含浸或塗佈於該基材之如[1]~[5]任一項之樹脂組成物。 [7] 一種覆金屬箔疊層板,具有:至少重疊了1片或2片以上之如[6]之預浸體;與疊層並成形在該預浸體之單面或兩面之金屬箔。 [8] 一種樹脂片,具有: 片狀基材;與塗佈在該片狀基材之單面或兩面並進行了乾燥的如[1]~[5]任一項之樹脂組成物。 [9] 一種印刷電路板,包含: 絕緣層;與形成在該絕緣層之單面或兩面之導體層; 該絕緣層含有如[1]~[5]任一項之樹脂組成物。 [發明之效果]
根據關於本發明之樹脂組成物,可獲得耐熱性優良且鍍敷密合性也優良之硬化物,而可達成鍍敷剝離強度優良之高性能之印刷電路板。
以下,針對本發明為了實施之形態(以下簡稱為「本實施形態」。)進行詳細地說明。以下之本實施形態係為了說明本發明之示例,本發明並非僅限定於以下之實施形態。本發明可在其要旨之範圍內適當地變形且實施。
<樹脂組成物> 本實施形態之樹脂組成物含有氰酸酯化合物(A)及下列通式(1)表示之環氧樹脂(B)(以下也簡稱為「環氧樹脂(B)」。); 【化2】式中,m及n各自獨立地表示1以上之整數。該通式(1)表示之環氧樹脂(B)也可為m及n各自獨立地代表不同整數之化合物之混合物。根據本實施形態之樹脂組成物,可達成鍍敷剝離強度優良之高性能之印刷電路板。其原因推測如下(但並非限定為此原因。)。本實施形態之樹脂組成物主要藉由含有通式(1)表示之環氧樹脂(B),環氧樹脂(B)的黏度較低,在樹脂組成物成形之時,對於基材或支持體等對象產生間隙之大小較小,故可獲得優良之鍍敷剝離強度。此外,本實施形態之樹脂組成物主要藉由含有氰酸酯化合物(A),玻璃轉化溫度高,可獲得耐熱性優良且鍍敷密合性也優良之硬化物。
<氰酸酯化合物(A)> 本實施形態之氰酸酯化合物(A)只要是分子內具有至少經1個氰氧基(氰酸酯基)取代之芳香族部分之樹脂即可,沒有特別之限定。藉由含有本實施形態之氰酸酯化合物(A),可獲得達成耐熱性優良之印刷電路板的樹脂組成物。其原因推測為藉由含有本實施形態之氰酸酯化合物(A),因此使樹脂組成物全體之玻璃轉化溫度變高,因此可獲得耐熱性更為優良之印刷電路板(但,並非限定為此原因。)。
就氰酸酯化合物(A)而言,可舉例如下列通式(2)表示之化合物。其中,氰酸酯化合物(A)可單獨使用1種或組合2種以上使用。 【化3】式中,Ar1
各自獨立地表示可具有取代基之伸苯基、可具有取代基之伸萘基或可具有取代基之伸聯苯基。Ra各自獨立地為選自氫原子、可具有取代基之碳數1~6之烷基、可具有取代基之碳數6~12之芳基、可具有取代基之碳數1~4之烷氧基、碳數1~6之烷基及碳數6~12之芳基鍵結而得之可具有取代基之芳烷基、或碳數1~6之烷基及碳數6~12之芳基鍵結而得之可具有取代基之烷芳基中之任一種。p表示與Ar1
鍵結之氰氧基的數目,為1~3之整數。q表示與Ar1
鍵結之Ra的數目,Ar1
是伸苯基時為4-p、伸萘基時為6-p、伸聯苯基時為8-p。t表示平均重複數,為0~50之整數,可為t不同之化合物的混合物。X各自獨立地為選自單鍵、碳數1~50之2價的有機基(氫原子可取代為鹵素原子)、氮原子數1~10之2價的有機基(-N-R-N-等)、羰基(-CO-)、羧基(-C(=O)O-)、二氧化羰基(-OC(=O)O-)、磺醯基(-SO2
-)、2價之硫原子或2價之氧原子中之任一種。
通式(2)之Ra表示之烷基,可具有鏈狀結構及環狀結構(環烷基等)之任一者。此外,通式(2)之Ra之烷基及芳基中的氫原子可取代為氟、氯等鹵素原子、甲氧基、苯氧基等烷氧基、氰基等。
就通式(2)之Ra之烷基的具體例而言,沒有特別之限定,可列舉甲基、乙基、丙基、異丙基、正丁基、異丁基、三級丁基、正戊基、1-乙基丙基、2,2-二甲基丙基、環戊基、己基、環己基及三氟甲基。
就通式(2)之Ra之芳基的具體例而言,沒有特別之限定,可列舉苯基、茬基、均三甲苯基、萘基、苯氧基苯基、乙基苯基、鄰、間或對氟苯基、二氯苯基、二氰基苯基、三氟苯基、甲氧基苯基、及鄰、間或對甲苯基。
就通式(2)之Ra之烷氧基之具體例而言,沒有特別之限定,可列舉甲氧基、乙氧基、丙氧基、異丙氧基、正丁氧基、異丁氧基、及三級丁氧基。
就通式(2)之X表示之2價之有機基的具體例而言,沒有特別之限定,可列舉亞甲基、伸乙基、三亞甲基、伸環戊基、伸環己基、三甲基伸環己基、聯苯基亞甲基、二甲基亞甲基-伸苯基-二甲基亞甲基、茀二基、及酞內酯二基。X表示之2價之有機基中之氫原子可取代為氟、氯等鹵素原子、甲氧基、苯氧基等烷氧基、氰基等。
就通式(2)之X之氮原子數1~10之2價之有機基而言,沒有特別之限定,可列舉亞胺基、聚醯亞胺基。
此外,就通式(2)中之X而言,可列舉具有下列通式(3)或下列通式(4)表示之結構的基。 【化4】式中,Ar2
各自獨立為選自伸苯基、伸萘基及伸聯苯基中之任一種。Rb、Rc、Rf、Rg各自獨立為選自氫原子、碳數1~6之烷基、碳數6~12之芳基、三氟甲基及經至少1個苯酚性羥基取代之芳基中之任一種。Rd、Re各自獨立為選自氫原子、碳數1~6之烷基、碳數6~12之芳基、碳數1~4之烷氧基及羥基中之任一種。u表示0~5之整數,可為不同u之化合物之混合物。 【化5】式中,Ar3
各自獨立為選自伸苯基、伸萘基或伸聯苯基之任一種。Ri、Rj各自獨立為選自氫原子、碳數1~6之烷基、碳數6~12之芳基、苄基、碳數1~4之烷氧基、羥基、三氟甲基及經至少1個氰氧基取代之芳基中之任一種。v表示0~5之整數,可為不同v之化合物之混合物。
就通式(3)之Ar2
及通式(4)之Ar3
的具體例而言,可列舉1,4-伸苯基、1,3-伸苯基、4,4’-伸聯苯基、2,4’-伸聯苯基、2,2’-伸聯苯基、2,3’-伸聯苯基、3,3’-伸聯苯基、3,4’-伸聯苯基、2,6-伸萘基、1,5-伸萘基、1,6-伸萘基、1,8-伸萘基、1,3-伸萘基、及1,4-伸萘基。
通式(3)之Rb~Rf及通式(4)之Ri、Rj之烷基及芳基與通式(2)所記載者相同。
就通式(2)表示之氰氧基取代芳香族化合物之具體例而言,可列舉氰氧基苯、1-氰氧基-2-、1-氰氧基-3-、或1-氰氧基-4-甲基苯、1-氰氧基-2-、1-氰氧基-3-、或1-氰氧基-4-甲氧基苯、1-氰氧基-2,3-、1-氰氧基-2,4-、1-氰氧基-2,5-、1-氰氧基-2,6-、1-氰氧基-3,4-或1-氰氧基-3,5-二甲基苯、氰氧基乙基苯、氰氧基丁基苯、氰氧基辛基苯、氰氧基壬基苯、2-(4-氰氧基苯基)-2-苯基丙烷(4-α-基酚之氰酸酯)、1-氰氧基-4-環己基苯、1-氰氧基-4-乙烯基苯、1-氰氧基-2-或1-氰氧基-3-氯苯、1-氰氧基-2,6-二氯苯、1-氰氧基-2-甲基-3-氯苯、氰氧基硝基苯、1-氰氧基-4-硝基-2-乙基苯、1-氰氧基-2-甲氧基-4-烯丙苯(丁香酚之氰酸酯)、甲基(4-氰氧基苯基)硫醚、1-氰氧基-3-三氟甲基苯、4-氰氧基聯苯、1-氰氧基-2-或1-氰氧基-4-乙醯基苯、4-氰氧基苯甲醛、4-氰氧基苯甲酸甲酯、4-氰氧基苯甲酸苯酯、1-氰氧基-4-乙醯胺基苯、4-氰氧基二苯基酮、1-氰氧基-2,6-二(三級丁基)苯、1,2-二氰氧基苯、1,3-二氰氧基苯、1,4-二氰氧基苯、1,4-二氰氧基-2-三級丁基苯、1,4-二氰氧基-2,4-二甲基苯、1,4-二氰氧基-2,3,4-三甲基苯、1,3-二氰氧基-2,4,6-三甲基苯、1,3-二氰氧基-5-甲基苯、1-氰氧基或2-氰氧基萘、1-氰氧基-4-甲氧基萘、2-氰氧基-6-甲基萘、2-氰氧基-7-甲氧基萘、2,2’-二氰氧基-1,1’-聯萘、1,3-、1,4-、1,5-、1,6-、1,7-、2,3-、2,6-或2,7-二氰氧基萘、2,2’-或4,4’-二氰氧基聯苯、4,4’-二氰氧基八氟聯苯、2,4’-或4,4’-二氰氧基二苯甲烷、雙(4-氰氧基-3,5-二甲基苯基)甲烷、1,1-雙(4-氰氧基苯基)乙烷、1,1-雙(4-氰氧基苯基)丙烷、2,2-雙(4-氰氧基苯基)丙烷、2,2-雙(4-氰氧基-3-甲基苯基)丙烷、2,2-雙(2-氰氧基-5-聯苯基)丙烷、2,2-雙(4-氰氧基苯基)六氟丙烷、2,2-雙(4-氰氧基-3,5-二甲基苯基)丙烷、1,1-雙(4-氰氧基苯基)丁烷、1,1-雙(4-氰氧基苯基)異丁烷、1,1-雙(4-氰氧基苯基)戊烷、1,1-雙(4-氰氧基苯基)-3-甲基丁烷、1,1-雙(4-氰氧基苯基)-2-甲基丁烷、1,1-雙(4-氰氧基苯基)-2,2-二甲基丙烷、2,2-雙(4-氰氧基苯基)丁烷、2,2-雙(4-氰氧基苯基)戊烷、2,2-雙(4-氰氧基苯基)己烷、2,2-雙(4-氰氧基苯基)-3-甲基丁烷、2,2-雙(4-氰氧基苯基)-4-甲基戊烷、2,2-雙(4-氰氧基苯基)-3,3-二甲基丁烷、3,3-雙(4-氰氧基苯基)己烷、3,3-雙(4-氰氧基苯基)庚烷、3,3-雙(4-氰氧基苯基)辛烷、3,3-雙(4-氰氧基苯基)-2-甲基戊烷、3,3-雙(4-氰氧基苯基)-2-甲基己烷、3,3-雙(4-氰氧基苯基)-2,2-二甲基戊烷、4,4-雙(4-氰氧基苯基)-3-甲基庚烷、3,3-雙(4-氰氧基苯基)-2-甲基庚烷、3,3-雙(4-氰氧基苯基)-2,2-二甲基己烷、3,3-雙(4-氰氧基苯基)-2,4-二甲基己烷、3,3-雙(4-氰氧基苯基)-2,2,4-三甲基戊烷、2,2-雙(4-氰氧基苯基)-1,1,1,3,3,3-六氟丙烷、雙(4-氰氧基苯基)苯基甲烷、1,1-雙(4-氰氧基苯基)-1-苯基乙烷、雙(4-氰氧基苯基)聯苯基甲烷、1,1-雙(4-氰氧基苯基)環戊烷、1,1-雙(4-氰氧基苯基)環己烷、2,2-雙(4-氰氧基-3-異丙基苯基)丙烷、1,1-雙(3-環己基-4-氰氧基苯基)環己烷、雙(4-氰氧基苯基)二苯基甲烷、雙(4-氰氧基苯基)-2,2-二氯乙烯、1,3-雙(2-(4-氰氧基苯基)-2-丙基)苯、1,4-雙(2-(4-氰氧基苯基)-2-丙基)苯、1,1-雙(4-氰氧基苯基)-3,3,5-三甲基環己烷、4-(雙(4-氰氧基苯基)甲基)聯苯、4,4-二氰氧基二苯基酮、1,3-雙(4-氰氧基苯基)-2-丙烷-1-酮、雙(4-氰氧基苯基)醚、雙(4-氰氧基苯基)硫醚、雙(4-氰氧基苯基)碸、4-氰氧基苯甲酸-4-氰氧基苯基酯(4-氰氧基苯基-4-氰氧基苯甲酸酯)、雙(4-氰氧基苯基)碳酸酯、1,3-雙(4-氰氧基苯基)金剛烷、1,3-雙(4-氰氧基苯基)-5,7-二甲基金剛烷、3,3-雙(4-氰氧基苯基)異苯并呋喃-1(3H)-酮(酚酞之氰酸酯)、3,3-雙(4-氰氧基-3-甲基苯基)異苯并呋喃-1(3H)-酮(鄰甲苯酚酞之氰酸酯)、9,9’-雙(4-氰氧基苯基)茀、9,9-雙(4-氰氧基-3-甲基苯基)茀、9,9-雙(2-氰氧基-5-聯苯基)茀、參(4-氰氧基苯基)甲烷、1,1,1-參(4-氰氧基苯基)乙烷、1,1,3-參(4-氰氧基苯基)丙烷、α,α,α’-參(4-氰氧基苯基)-1-乙基-4-異丙基苯、1,1,2,2-肆(4-氰氧基苯基)乙烷、肆(4-氰氧基苯基)甲烷、2,4,6-參(N-甲基-4-氰氧基苯胺基)-1,3,5-三氮、2,4-雙(N-甲基-4-氰氧基苯胺基)-6-(N-甲基苯胺基)-1,3,5-三氮、雙(N-4-氰氧基-2-甲基苯基)-4,4’-氧基二酞醯亞胺、雙(N-3-氰氧基-4-甲基苯基)-4,4’-氧基二酞醯亞胺、雙(N-4-氰氧基苯基)-4,4’-氧基二酞醯亞胺、雙(N-4-氰氧基-2-甲基苯基)-4,4’-(六氟亞異丙基)二酞醯亞胺、參(3,5-二甲基-4-氰氧基苄基)異氰尿酸酯、2-苯基-3,3-雙(4-氰氧基苯基)苄甲內醯胺、2-(4-甲基苯基)-3,3-雙(4-氰氧基苯基)苄甲內醯胺、2-苯基-3,3-雙(4-氰氧基-3-甲基苯基)苄甲內醯胺、1-甲基-3,3-雙(4-氰氧基苯基)吲哚啉-2-酮、2-苯基-3,3-雙(4-氰氧基苯基)吲哚啉-2-酮、苯酚酚醛清漆型氰酸酯化合物、甲酚酚醛清漆型氰酸酯化合物、三苯酚酚醛清漆型氰酸酯化合物、茀酚醛清漆型氰酸酯化合物、苯酚芳烷基型氰酸酯化合物、甲酚芳烷基型氰酸酯化合物、萘酚芳烷基型氰酸酯化合物、聯苯芳烷基型氰酸酯化合物、苯酚改性二甲苯甲醛型氰酸酯化合物、改性萘甲醛型氰酸酯化合物、苯酚改性二環戊二烯型氰酸酯化合物、及具有聚伸萘基醚結構之苯酚樹脂的氰酸酯化合物。此等氰酸酯化合物(A)可單獨使用1種或2種以上併用。
其中,就苯酚酚醛清漆型氰酸酯化合物、甲酚酚醛清漆型氰酸酯化合物而言,可列舉藉由公知方法將苯酚酚醛清漆樹脂或甲酚酚醛清漆樹脂進行氰酸酯化而得者。就苯酚酚醛清漆樹脂或甲酚酚醛清漆樹脂而言,可列舉藉由公知方法將苯酚、烷基取代之苯酚或鹵素取代之苯酚與福馬林(formalin)或聚甲醛等甲醛化合物於酸性溶液中使其反應而得者。
就三苯酚酚醛清漆型氰酸酯化合物而言,可列舉藉由公知方法使三苯酚酚醛清漆樹脂進行氰酸酯化而得者。就三苯酚酚醛清漆樹脂而言,可列舉將羥苯甲醛與苯酚在酸性觸媒之存在下使其反應而得者。
就茀酚醛清漆型氰酸酯化合物而言,可列舉藉由公知方法,使茀酚醛清漆樹脂進行氰酸酯化而得者。就茀酚醛清漆樹脂而言,可列舉將茀酮化合物與9,9-雙(羥芳基)茀類在酸性觸媒之存在下使其反應而得者。
就苯酚芳烷基型氰酸酯化合物、甲酚芳烷基型氰酸酯化合物、萘酚芳烷基型氰酸酯化合物、聯苯芳烷基型氰酸酯化合物而言,可列舉,藉由公知方法使苯酚芳烷基樹脂、甲酚芳烷基樹脂、萘酚芳烷基樹脂或聯苯芳烷基樹脂進行氰酸酯化而得者。就苯酚芳烷基樹脂、甲酚芳烷基樹脂、萘酚芳烷基樹脂或聯苯芳烷基樹脂而言,可列舉藉由公知方法,將如Ar2
-(CH2
Y)2
表示之雙鹵素甲基化合物與苯酚化合物在酸性觸媒或無觸媒下使其反應而得者;將如Ar2
-(CH2
OR)2
表示之雙(烷氧基甲基)化合物或如Ar2
-(CH2
OH)2
表示之雙(羥甲基)化合物與苯酚化合物在酸性觸媒之存在下使其反應而得者;或將芳香族醛化合物、芳烷基化合物、苯酚化合物縮聚而得者。
就苯酚改性二甲苯甲醛型氰酸酯化合物而言,可列舉藉由公知方法,將苯酚改性二甲苯甲醛樹脂進行氰酸酯化而得者。就苯酚改性二甲苯甲醛樹脂而言,可列舉藉由公知方法,使二甲苯甲醛樹脂與苯酚化合物在酸性觸媒之存在下使其反應而得者。
就改性萘甲醛型氰酸酯化合物而言,可列舉藉由公知方法使改性萘甲醛樹脂進行氰酸酯化而得者。就改性萘甲醛樹脂而言,可列舉藉由公知方法,使萘甲醛樹脂與羥基取代芳香族化合物在酸性觸媒之存在下使其反應而得者。
就苯酚改性二環戊二烯型氰酸酯化合物、具有聚伸萘基醚結構之苯酚樹脂的氰酸酯化合物而言,可列舉藉由公知方法使苯酚改性二環戊二烯樹脂、具有聚伸萘基醚結構之苯酚樹脂進行氰酸酯化而得者。就苯酚改性二環戊二烯樹脂、具有聚伸萘基醚結構之苯酚樹脂而言,可列舉藉由公知方法將1分子中具有2個以上之苯酚性羥基的多價羥萘化合物在鹼性觸媒之存在下使其脫水縮合而得者。
上述中,宜為苯酚酚醛清漆型氰酸酯化合物、萘酚芳烷基型氰酸酯化合物、聯苯芳烷基型氰酸酯化合物、伸萘基醚型氰酸酯化合物、二甲苯樹脂型氰酸酯化合物、及金剛烷骨架型氰酸酯化合物,更宜為萘酚芳烷基型氰酸酯化合物。
從使用了此等之氰酸酯化合物(A)之樹脂組成物而獲得之硬化物,因為玻璃轉化溫度高,故耐熱性優良且鍍敷密合性也優良。特別是從使用了萘酚芳烷基型氰酸酯化合物之樹脂組成物而獲得之硬化物,耐熱性與鍍敷密合性的平衡良好。
氰酸酯化合物(A)之含量可因應期望之特性適當設定,雖然沒有特別之限制,相對於樹脂組成物中之樹脂固體成分的總量(100質量份),宜為1~90質量份,更宜為10~85質量份,進一步宜為30~75質量份,尤其宜為40~60質量份。藉由使氰酸酯化合物(A)之含量為1質量份以上,有可獲得更優良之耐熱性之趨勢,此外,藉由使氰酸酯化合物(A)之含量為90質量份以下,有可獲得更優良之鍍敷剝離強度之趨勢。此處,若無特別指明之情況,「樹脂組成物中之樹脂固體成分」係指樹脂組成物中扣除溶劑、填充材(C)等樹脂以外之成分後的成分,「樹脂固體成分之總量」係指樹脂組成物扣除溶劑、填充材(C)等樹脂以外之成分後的合計量。
通式(1)表示之環氧樹脂(B)之黏度,雖然沒有特別之限定,宜為10mPa・s/25℃以上20000 mPa・s/25℃以下,更宜為100 mPa・s/25℃以上10000 mPa・s/25℃以下,進一步宜為500 mPa・s/25℃以上5000 mPa・s/25℃以下,尤其宜為1000 mPa・s/25℃以上2500 mPa・s/25℃以下。藉由使黏度為上述範圍內,有可獲得更優良之鍍敷剝離強度的趨勢。黏度如上述範圍內之環氧樹脂(B)可適當選擇市面販售者,也可組合此等市面販售者。
通式(1)表示之環氧樹脂(B)只要是通式(1)表示者即可,沒有特別之限定,可使用市面販售者,例如宜為ADEKA(股)公司製商品名「EP-4000S」。
如通式(1)表示之環氧樹脂(B)之含量可因應期望之特性適當設定,雖然沒有特別之限制,相對於樹脂組成物中樹脂固體成分之總量(100質量份),宜為1~90質量份,更宜為20~75質量份,進一步宜為40~60質量份,尤其宜為40~60質量份。藉由使環氧樹脂(B)之含量為1質量份以上,有可獲得更優良之鍍敷剝離強度的趨勢,此外,藉由使環氧樹脂(B)之含量為90質量份以下,有可獲得更優良之耐熱性的趨勢。
<填充材(C)> 本實施形態之樹脂組成物宜更含有填充材(C)。藉由含有填充材(C),可更確實地發揮本發明之作用效果,有可獲得優良之鍍敷剝離強度的趨勢。此外,可更確實地發揮本實施形態之氰酸酯化合物(A)之作用效果,也有可獲得優良之耐熱性的趨勢。
就填充材(C)而言,可適用公知者,其種類沒有特別之限定,可適當使用該業界中一般所使用者。具體而言,可列舉天然二氧化矽、熔融二氧化矽、合成二氧化矽、非晶二氧化矽、Aerosil、中空二氧化矽等二氧化矽類、白碳、鈦白、氧化鋅、氧化鎂、氧化鋯、氮化硼、凝聚氮化硼、氮化矽、氮化鋁、硫酸鋇、氫氧化鋁、氫氧化鋁加熱處理品(氫氧化鋁經加熱處理除去一部分結晶水者)、水鋁石、氫氧化鎂等金屬水合物、氧化鉬或鉬酸鋅等之鉬化合物、硼酸鋅、錫酸鋅、氧化鋁、黏土、高嶺土、滑石、煅燒黏土、煅燒高嶺土、煅燒滑石、雲母、E-玻璃、A-玻璃、NE-玻璃、C-玻璃、L-玻璃、D-玻璃、S-玻璃、M-玻璃G20、玻璃短纖維(包含E玻璃、T玻璃、D玻璃、S玻璃、Q玻璃等玻璃微粉末類。)、中空玻璃、球狀玻璃等無機系之填充材,其他還有苯乙烯型、丁二烯型、丙烯酸型等橡膠粉末、核殼(core shell)型之橡膠粉末、矽酮樹脂粉末、矽酮橡膠粉末、矽酮複合粉末等有機系之填充材。此等填充材(C)可單獨使用1種或組合2種以上使用。
藉由含有此等之填充材(C),有樹脂組成物之鍍敷剝離強度、熱膨脹特性、尺寸安定性、阻燃性等特性更為提升之趨勢。
本實施形態之樹脂組成物中填充材(C)之含量可因應期望之特性適當設定,雖然沒有特別之限定,相對於樹脂組成物中樹脂固體成分之總量(100質量份),宜為50~1600質量份,更宜為60~1000質量份,進一步宜為70~500質量份,尤其宜為80~200質量份。藉由使填充材(C)之含量為50~1600質量份,有樹脂組成物之成形性變得良好之趨勢。
此處使用填充材(C)時,宜與矽烷偶聯劑或濕潤分散劑併用。就矽烷偶聯劑而言,可適用一般於無機物之表面處理中所使用者,其種類沒有特別之限定。具體而言可列舉γ-胺丙基三乙氧基矽烷、N-β-(胺乙基)-γ-胺丙基三甲氧基矽烷等胺基矽烷系、γ-環氧丙氧基丙基三甲氧基矽烷、β-(3,4-環氧基環己基)乙基三甲氧基矽烷等環氧矽烷系、γ-甲基丙烯醯氧丙基三甲氧基矽烷、乙烯-三(β-甲氧基乙氧基)矽烷等乙烯矽烷系、N-β-(N-乙烯苄基胺乙基)-γ-胺丙基三甲氧基矽烷鹽酸鹽等陽離子矽烷系、及苯基矽烷系。矽烷偶聯劑可單獨使用1種或組合2種以上使用。此外,就濕潤分散劑而言,可適用一般塗料用中所使用者,其種類沒有特別之限定。宜使用共聚合系之濕潤分散劑,就具體例而言可列舉BYK Japan(股)製的Disperbyk-110、111、161、180、BYK-W996、BYK-W9010、BYK-W903、BYK-W940。濕潤分散劑可單獨使用1種或組合2種以上使用。
<其他成分> 另外,本實施形態之樹脂組成物可因應需求含有其他成分。就其他成分而言,雖然沒有特別之限定,可舉例如選自於由上述環氧樹脂(B)以外之環氧樹脂(以下稱為「其他之環氧樹脂」。)、馬來醯亞胺化合物、苯酚樹脂、氧雜環丁烷樹脂、苯并
化合物、及具有可聚合之不飽和基之化合物構成之群組中之任1種類以上。藉由使用如此之其他成分,可提升樹脂組成物硬化後之硬化物的阻燃性、低介電性等期望之特性。
就其它之環氧樹脂而言,只要是不具有通式(1)表示之結構單元者,為1分子中具有2個以上之環氧基之環氧樹脂即可,可適用公知者,其種類沒有特別之限定。具體而言,可列舉雙酚A型環氧樹脂、雙酚E型環氧樹脂、雙酚F型環氧樹脂、雙酚S型環氧樹脂、苯酚酚醛清漆型環氧樹脂、雙酚A酚醛清漆型環氧樹脂、環氧丙基酯型環氧樹脂、芳烷基酚醛清漆型環氧樹脂、聯苯芳烷基型環氧樹脂、伸萘基醚型環氧樹脂、甲酚酚醛清漆型環氧樹脂、多官能苯酚型環氧樹脂、萘型環氧樹脂、蒽型環氧樹脂、萘骨架改性酚醛清漆型環氧樹脂、苯酚芳烷基型環氧樹脂、萘酚芳烷基型環氧樹脂、二環戊二烯型環氧樹脂、聯苯型環氧樹脂、脂環式環氧樹脂、多元醇型環氧樹脂、含磷環氧樹脂、環氧丙基胺、環氧丙酯、使丁二烯等之雙鍵環氧化而得之化合物、及藉由將含羥基之矽酮樹脂類與表氯醇反應而獲得之化合物。此等之其他之環氧樹脂中,宜為聯苯芳烷基型環氧樹脂、伸萘基醚型環氧樹脂、多官能苯酚型環氧樹脂、及萘型環氧樹脂。藉由使用如此之其他之環氧樹脂,有阻燃性及耐熱性更為提升之趨勢。此等之環氧樹脂可單獨使用1種或組合2種以上使用。
就馬來醯亞胺化合物而言,只要是1分子中具有1個以上之馬來醯亞胺基之化合物即可,可使用一般之公知者,其種類沒有特別之限定。具體而言可列舉,4,4-二苯基甲烷雙馬來醯亞胺、苯基甲烷馬來醯亞胺、間伸苯基雙馬來醯亞胺、2,2-雙(4-(4-馬來醯亞胺苯氧基)-苯基)丙烷、3,3-二甲基-5,5-二乙基-4,4-二苯基甲烷雙馬來醯亞胺、4-甲基-1,3-伸苯基雙馬來醯亞胺、1,6-雙馬來醯亞胺-(2,2,4-三甲基)己烷、4,4-二苯基醚雙馬來醯亞胺、4,4-二苯基碸雙馬來醯亞胺、1,3-雙(3-馬來醯亞胺苯氧基)苯、1,3-雙(4-馬來醯亞胺苯氧基)苯、聚苯基甲烷馬來醯亞胺、酚醛清漆型馬來醯亞胺、聯苯芳烷基型馬來醯亞胺、及此等馬來醯亞胺化合物之預聚物、以及馬來醯亞胺化合物與胺化合物之預聚物。此等之中,以酚醛清漆型馬來醯亞胺化合物、及聯苯芳烷基型馬來醯亞胺化合物較為理想。此等馬來醯亞胺化合物可單獨使用1種或組合2種以上使用。
就苯酚樹脂而言,只要是1分子中具有2個以上之羥基之苯酚樹脂即可,可使用一般公知者,其種類沒有特別之限定。具體而言,可列舉雙酚A型苯酚樹脂、雙酚E型苯酚樹脂、雙酚F型苯酚樹脂、雙酚S型苯酚樹脂、苯酚酚醛清漆樹脂、雙酚A酚醛清漆型苯酚樹脂、環氧丙基酯型苯酚樹脂、芳烷基酚醛清漆型苯酚樹脂、聯苯芳烷基型苯酚樹脂、甲酚酚醛清漆型苯酚樹脂、多官能苯酚樹脂、萘酚樹脂、萘酚酚醛清漆樹脂、多官能萘酚樹脂、蒽型苯酚樹脂、萘骨架改性酚醛清漆型苯酚樹脂、苯酚芳烷基型苯酚樹脂、萘酚芳烷基型苯酚樹脂、二環戊二烯型苯酚樹脂、聯苯型苯酚樹脂、脂環式苯酚樹脂、多元醇型苯酚樹脂、含磷苯酚樹脂、及含羥基之矽酮樹脂類。此等之苯酚樹脂中,聯苯芳烷基型苯酚樹脂、萘酚芳烷基型苯酚樹脂、含磷苯酚樹脂、及含羥基之矽酮樹脂以其阻燃性的點而較為理想。此等之苯酚樹脂可單獨使用1種或組合2種以上使用。
就氧雜環丁烷樹脂而言,可使用一般公知者,其種類沒有特別之限定。具體而言可列舉氧雜環丁烷、2-甲基氧雜環丁烷、2,2-二甲基氧雜環丁烷、3-甲基氧雜環丁烷、3,3-二甲基氧雜環丁烷等烷基氧雜環丁烷、3-甲基-3-甲氧基甲基氧雜環丁烷、3,3-二(三氟甲基)全氟氧雜環丁烷、2-氯甲基氧雜環丁烷、3,3-雙(氯甲基)氧雜環丁烷、聯苯型氧雜環丁烷、OXT-101(東亞合成製商品名)、及OXT-121(東亞合成製商品名)。此等之氧雜環丁烷樹脂可單獨使用1種或2種以上併用。
就苯并
化合物而言,只要是1分子中具有2個以上之二氫苯并
環之化合物即可,可使用一般公知者,其種類沒有特別之限定。具體而言,可列舉雙酚A型苯并
BA-BXZ(小西化學製商品名)、雙酚F型苯并
BF-BXZ(小西化學製商品名)、及雙酚S型苯并
BS-BXZ(小西化學製商品名)。此等之苯并
化合物可單獨使用1種或2種以上併用。
就具有可聚合之不飽和基之化合物而言,可使用一般公知者,其種類沒有特別之限定。具體而言,可列舉乙烯、丙烯、苯乙烯、二乙烯苯、二乙烯聯苯等乙烯化合物、(甲基)丙烯酸甲酯、(甲基)丙烯酸-2-羥基乙酯、(甲基)丙烯酸-2-羥基丙酯、二(甲基)丙烯酸聚丙二醇酯、三羥甲基丙烷二(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、四(甲基)丙烯酸新戊四醇酯、六(甲基)丙烯酸二新戊四醇酯等1元或多元醇之(甲基)丙烯酸酯類、雙酚A型環氧(甲基)丙烯酸酯、雙酚F型環氧(甲基)丙烯酸酯等環氧(甲基)丙烯酸酯類、苯并環丁烯樹脂、及(雙)馬來醯亞胺樹脂。此等之具有不飽和基之化合物可單獨使用1種或2種以上併用。
此外,本實施形態之樹脂組成物因應需求可更含有為了適當調節硬化速度之硬化促進劑。就此硬化促進劑而言,可適用作為氰酸酯化合物或環氧樹脂等之硬化促進劑之一般所使用者,其種類沒有特別之限定。就其具體例而言,可列舉辛酸鋅、環烷酸鋅、環烷酸鈷、環烷酸銅、乙醯丙酮鐵、辛酸鎳、辛酸錳等有機金屬鹽類、苯酚、茬酚、甲酚、間苯二酚、兒茶酚、辛基苯酚、壬基苯酚等苯酚化合物、1-丁醇、2-乙基己醇等醇類、2-甲基咪唑、2-乙基-4-甲基咪唑、2-苯基咪唑、1-氰基乙基-2-苯基咪唑、1-氰基乙基-2-乙基-4-甲基咪唑、2-苯基-4,5-二羥基甲基咪唑、2-苯基-4-甲基-5-羥基甲基咪唑等咪唑類及此等咪唑類之羧酸或其酸酐類之加成物等衍生物、二氰基二醯胺、苄基二甲基胺、4-甲基-N,N-二甲基苄基胺等胺類、膦系化合物、氧化膦系化合物、鏻鹽系化合物、二膦系化合物等磷化合物、環氧-咪唑加成物系化合物、過氧化苯甲醯、對氯過氧化苯甲醯、二(三級丁基)過氧化物、過氧化碳酸二異丙酯、過氧化碳酸二-2-乙基己酯等過氧化物、及偶氮雙異丁腈等偶氮化合物。硬化促進劑可單獨使用1種或組合2種以上使用。
硬化促進劑之含量可考慮樹脂之硬化度或樹脂組成物之黏度等適當調整,雖然沒有特別之限定,相對於樹脂組成物中之樹脂固體成分的總量(100質量份),宜為0.005~10質量份。
另外,本實施形態之樹脂組成物,於不損及期望之特性的範圍,可與其他之熱固性樹脂、熱塑性樹脂、其寡聚合物、彈性體類等各種之高分子化合物、阻燃性化合物、各種添加劑等併用。只要是此等物質之一般所使用者即可,並沒有特別之限定。例如,就阻燃性化合物之具體例而言,可列舉4,4’-二溴聯苯等溴化合物、磷酸酯、磷酸三聚氰胺、含磷環氧樹脂、三聚氰胺或苯胍胺等氮化合物、含
環之化合物、及矽酮系化合物。此外,就各種添加劑而言,可列舉紫外線吸收劑、抗氧化劑、光聚合起始劑、螢光增白劑、光敏劑、染料、顏料、增黏劑、流動調整劑、潤滑劑、消泡劑、分散劑、塗平劑、光澤劑、聚合抑制劑等。此等物質可因應期望單獨使用1種或組合2種以上使用。
其中,本實施形態之樹脂組成物,因應需求可含有有機溶劑。此時,本發明之樹脂組成物可作為將上述之各種樹脂成分至少一部分,宜為全部,溶解於有機溶劑或相溶於有機溶劑之態樣(溶液或清漆)來使用。就有機溶劑而言,只要是可將上述之各種樹脂成分之至少一部分,宜為全部,溶解或可相溶者即可,可適用公知者,其種類沒有特別之限制。具體而言可列舉丙酮、甲乙酮、甲基異丁酮等酮類、丙二醇一甲基醚、丙二醇一甲醚醋酸酯等賽珞蘇(cellosolve)系溶劑、乳酸乙酯、乙酸甲酯、乙酸乙酯、乙酸丁酯、乙酸異戊酯、甲氧基丙酸甲酯、羥基異丁酸甲酯等酯系溶劑、二甲基乙醯胺、二甲基甲醯胺等醯胺類等極性溶劑類、甲苯、二甲苯等芳香族烴等非極性溶劑。此等有機溶劑可單獨使用1種或組合2種以上使用。
<樹脂組成物之製造方法> 本實施形態之樹脂組成物可依循通常方法製造,只要是可獲得均勻含有氰酸酯化合物(A)、通式(1)表示之環氧樹脂(B)及上述之其他任意成分的樹脂組成物之方法即可,其製備方法並沒有特別之限定。例如可將氰酸酯化合物(A)及通式(1)表示之環氧樹脂(B)依序摻合至溶劑中,充分攪拌後可輕易製備本實施形態之樹脂組成物。
其中,製備樹脂組成物時,可進行為了使各成分均勻地溶解或分散之公知的處理(攪拌、混合、混練處理等)。例如,在均勻分散填充材(C)時,藉由使用具有適當攪拌能力之攪拌機所設置之攪拌槽進行攪拌分散處理,可提高對於樹脂組成物之分散性。上述之攪拌、混合、混練處理可使用例如球磨機、珠粒磨機等以混合為目的之裝置,或公轉自轉型之混合裝置等公知的裝置來適當地進行。
本實施形態之樹脂組成物係沒有特別之限制,可作為印刷電路板之絕緣層用材料、半導體封裝體用材料使用。例如可將本實施形態之樹脂組成物溶解於溶劑而得之溶液含浸或塗布於基材並進行乾燥而成為預浸體。
此外,使用可剝離之塑膠薄膜作為支持體,藉由將本實施形態之樹脂組成物溶解於溶劑而得之溶液塗布於塑膠薄膜並進行乾燥後可成為樹脂片。樹脂片可使用作為增建用薄膜或乾膜阻焊膜。此處,溶劑可於20℃~150℃之溫度加熱1~90分鐘而乾燥。此外,樹脂組成物可於只乾燥溶劑之未硬化之狀態使用,也可因應需求成為半硬化(B階段化)之狀態後使用。
<預浸體> 以下,針對本實施形態之預浸體進行詳細描述。本實施形態之預浸體具有:基材;及含浸或塗布於該基材之上述本實施形態之樹脂組成物。預浸體之製造方法只要是組合本實施形態之樹脂組成物與基材以製造預浸體之方法即可,沒有特別之限制,可將本實施形態之樹脂組成物含浸或塗布於基材而獲得預浸體。更具體而言,將本實施形態之樹脂組成物含浸或塗布於基材後,藉由於120~220℃進行乾燥2~15分鐘左右之方法等使其半硬化後,可製造本實施形態之預浸體。此時,樹脂組成物相對於基材之附著量,也就是樹脂組成物的量(包含填充材(C)。)相對於半硬化後之預浸體之總量(100質量份)宜為20~99質量份之範圍。
就本實施形態之基材而言,雖然沒有特別之限定,例如可使用各種印刷電路板材料中所使用之公知者。具體而言,可列舉E玻璃、D玻璃、L玻璃、S玻璃、T玻璃、Q玻璃、UN玻璃、NE玻璃、球狀玻璃等玻璃纖維;石英等玻璃以外的無機纖維;聚醯亞胺、聚醯胺、聚酯等有機纖維;液晶聚酯等織布。就基材之形狀而言,已知有織布、不織布、粗紗、切股氈(chopped strand mat)、表面氈(surfacing mat)等,可為任一者皆無影響。基材可單獨使用1種或組合2種以上使用。此外,基材之厚度雖然沒有特別之限定,若作為疊層板用途宜為0.01~0.2mm之範圍,考慮尺寸安定性之觀點,尤其適宜為經施以超開纖處理或孔目堵塞處理之織布。另外,考慮吸濕耐熱性之觀點,以經環氧矽烷處理、胺基矽烷處理等矽烷偶聯劑等表面處理之玻璃織布較為理想。此外,考慮電特性之方面,液晶聚酯織布較為理想。
<覆金屬箔疊層板> 本實施形態之覆金屬箔疊層板具有:重疊1片或2片以上之上述之預浸體;與疊層並成形在該預浸體之單面或兩面之金屬箔。具體而言,可將上述之預浸體之一片或重疊之數片,於其單面或兩面配置銅或鋁等金屬箔,藉由疊層並成形來製造。此處使用之金屬箔只要是印刷電路板材料中所使用者即可,雖然沒有特別之限定,宜為壓延銅箔或電解銅箔等銅箔。此外,金屬箔之厚度,雖然沒有特別之限定,宜為2~70μm,更宜為3~35μm。就成形條件而言,可適用通常之印刷電路板用疊層板及多層板之方法。例如,藉由使用多段壓合機、多段真空壓合機、連續成形機、高壓釜成形機等,於溫度180~350℃、加熱時間100~300分鐘、表面壓力20~100kg/cm2
進行疊層並成形可製造本實施形態之覆金屬箔疊層板。此外,藉由將上述之預浸體與另外製作之內層用電路板組合且疊層並成形,也可成為多層板。就多層板之製造方法而言,例如於上述之預浸體1片之兩面配置35μm之銅箔,以上述條件疊層並形成後,形成內層電路,該電路實施黑化處理而形成內層電路板,之後將此內層電路板與上述之預浸體1片片地交替配置,更於最外層配置銅箔,藉由於上述條件下,宜為於真空下進行疊層並成形,可製作多層板。
而,本實施形態之覆金屬箔疊層板可適用作為印刷電路板。印刷電路板可依循通常方法製造,其製造方法沒有特別之限定。以下展示印刷電路板之製造方法的一例。首先準備上述之覆銅疊層板等之覆金屬箔疊層板。接著,於覆金屬箔疊層板之表面施以蝕刻處理形成內層電路以製作內層基板。於該內層基板之內層電路表面,因應需求進行為了提高密合強度的表面處理,接著於該內層電路表面重疊所需之上述預浸體片數,進一步於其外側疊層外層電路用的金屬箔,經加熱加壓而一體成形。以如此方式製造內層電路與外層電路用之金屬箔之間形成了基材及由熱固性樹脂組成物之硬化物構成之絕緣層的多層之疊層板。接下來於該多層之疊層板施以通孔(through hole)或介層孔(via hole)用之穿孔加工後,於此孔之壁面形成使內層電路與外層電路用之金屬箔導通之鍍敷金屬皮膜,進一步地藉由於外層電路用之金屬箔施以蝕刻處理形成外層電路,以製造印刷電路板。
<印刷電路板> 本實施形態之印刷電路板包含:絕緣層;與形成在該絕緣層之單面或兩面之導體層;該絕緣層含有上述之本實施形態之樹脂組成物。也就是說,上述之本實施形態之預浸體(基材及含浸或塗布於該基材之本實施形態之樹脂組成物),上述之本實施形態之覆金屬箔疊層板之樹脂組成物之層(由本實施形態之樹脂組成物構成之層)為含有本實施形態之樹脂組成物之絕緣層所構成而成。
<樹脂片> 本實施形態之樹脂片具有:片狀基材;與塗布在該片狀基材之單面或兩面並進行了乾燥的上述本實施形態之樹脂組成物。樹脂片可藉由將溶解於溶劑而得之溶液(樹脂組成物)塗布(塗覆)於片狀基材並進行乾燥而獲得。就此處使用之片狀基材而言,可舉例如聚乙烯薄膜、聚丙烯薄膜、聚碳酸酯薄膜、聚對苯二甲酸乙二醇酯薄膜、乙烯四氟乙烯共聚合物薄膜、及於此等之薄膜的表面塗布了離型劑之離型薄膜、聚醯亞胺薄膜等有機系薄膜基材、銅箔、鋁箔等導體箔、玻璃板、SUS板、FRP等板狀者,並沒有特別之限定。就塗布方法而言,可舉例如將本實施形態之樹脂組成物溶解於溶劑後而得之溶液,以塗布棒、模塗布機、刮刀片、BAKER式塗膜器等塗布於支持體上之方法。此外,乾燥後,藉由將支持體從疊層片剝離或蝕刻,也可成為單層片(樹脂片)。其中,藉由將使上述本實施形態之樹脂組成物溶解於溶劑而得之溶液供給至具有片狀之模槽的模具內並進行乾燥等使其成形為片狀,也可不使用支持體而獲得單層片(樹脂片)。
其中,本實施形態之單層或疊層片之製作中,除去溶劑時之乾燥條件雖然沒有特別之限定,若為低溫則樹脂組成物中溶劑容易殘留,若為高溫則會使樹脂組成物進行硬化,故宜為於20℃~200℃之溫度乾燥1~90分鐘。此外,本實施形態之單層片或疊層片之樹脂層之厚度可藉由本實施形態之樹脂組成物的溶液濃度與塗布厚度進行調整,雖然並沒有特別之限制,一般而言若塗布厚度厚會使乾燥時溶劑容易殘留,故宜為0.1~500μm。 [實施例]
以下將展示合成例、實施例及比較例來更詳細地說明本發明,但本發明並非僅限定於此等示例。
(合成例1)氰酸酯化合物之合成 將1-萘酚芳烷基樹脂(新日鐵住金化學(股)公司製)300g(OH基換算1.28mol)及三乙胺194.6g(1.92mol)(相對於羥基1mol為1.5mol)溶解於二氯甲烷1800g,令其為溶液1。
將氯化氰125.9g(2.05mol)(相對於羥基1mol為1.6mol)、二氯甲烷293.8g、36%鹽酸194.5g(1.92mol)(相對於羥基1mol為1.5mol)、水1205.9g在攪拌下保持於液溫-2~-0.5℃的同時,花費30分鐘滴加溶液1。溶液1滴加結束後,於同溫度攪拌30分鐘後,花費10分鐘滴加將三乙胺65g(0.64mol)(相對於羥基1mol為0.5mol)溶解於二氯甲烷65g而得之溶液(溶液2)。溶液2滴加結束後,於同溫度攪拌30分鐘完成反應。
之後將反應液靜置使有機相與水相分離。獲得之有機相以水1300g清洗5次,水洗第5次的廢水的電傳導度為5μS/cm,確認藉由水之清洗,已充分除去可除去之離子性化合物。
水洗後之有機相在減壓下濃縮,最後於90℃濃縮1小時乾燥固化而獲得目的之萘酚芳烷基型之氰酸酯化合物(SNCN)(橙色黏性物)331g。獲得之SNCN之質量平均分子量Mw為600。此外,SNCN之IR譜顯示有2250cm-1
(氰酸酯基)之吸收,且未顯示羥基之吸收。
(實施例1) 將藉由合成例1獲得之SNCN50質量份、下列通式(1)表示之環氧樹脂(EP-4000S,黏度:1800mPa・s/25℃,ADEKA(股)製)50質量份、熔融二氧化矽(SC2050MB,Admatechs.製)100質量份、辛酸鋅(日本化學產業(股)製)0.15質量份混合而獲得清漆。此清漆以甲乙酮稀釋,含浸塗布於厚度0.1mm之E玻璃織布,於150℃加熱5分鐘進行乾燥,獲得樹脂含量50質量%之預浸體。
重疊8片獲得之預浸體並於上下配置12μm厚之電解銅箔(3EC-M3-VLP,三井金屬(股)製),在壓力30kgf/cm2
、溫度220℃進行120分鐘之疊層並成形,獲得絕緣層厚度0.8mm之覆金屬箔疊層板。使用獲得之覆金屬箔疊層板進行鍍敷剝離強度、彎曲彈性係數及介電係數之評價。評價結果表示於表1。
(比較例1) 於實施例1中,使用聯苯芳烷基型環氧樹脂(NC-3000-FH,日本化藥(股)製)50質量份替代通式(1)表示之環氧樹脂50質量份,且辛酸鋅使用0.12質量份以外,以與實施例1相同方法獲得厚度0.8mm之覆金屬箔疊層板。獲得之覆金屬箔疊層板之各評價結果表示於表1。
(測定方法及評價方法) 鍍敷剝離強度:將實施例1及比較例1獲得之絕緣層厚度0.8mm之覆金屬箔疊層板經上村工業製之無電解銅鍍敷程序(使用藥液名:MCD-PL、MDP-2、MAT-SP、MAB-4-C、MEL-3-APEA ver.2),施以約0.8μm之無電解銅鍍敷,於130℃進行乾燥1小時。接著,施以電解銅鍍敷使鍍敷銅之厚度成為18μm,於180℃進行乾燥1小時。以如此方式製作絕緣層上形成厚度18μm之導體層(鍍敷銅)之樣本並進行評價。鍍敷銅之黏著力係依循JIS C6481測定3次,求其平均值。
彎曲彈性係數:藉由蝕刻除去於實施例1及比較例1獲得之絕緣層厚度0.8mm之覆金屬箔疊層板之兩面的銅箔後,依循JIS C6481,藉由使用試驗片(50mm×25mm×0.8mm)、試驗數5以測定彎曲強度彈性係數,求其最大值之平均值。
介電係數(Dk):使用藉由蝕刻除去了實施例1及比較例1獲得之絕緣層厚度0.8mm之覆金屬箔疊層板的銅箔後而獲得之試驗片,以空腔共振器擾動法(Agilent 8722ES,Agilent Technology製)實施1GHz之介電係數之測定3次,求其平均値。
從表1可明顯地至少確認到,藉由使用實施例之樹脂組成物,可達成鍍敷剝離強度優良之預浸體及印刷電路板等。
本申請案係基於2015年4月28日向日本專利局提申之日本專利申請案(日本特願2015-091041號),其內容納入於此作為參考。 [產業上利用性]
如同以上說明,關於本發明之樹脂組成物,於電氣電子材料、機具材料、航空材料等之各種用途,例如作為電絕緣材料、半導體塑膠封裝體、密封材料、黏著劑、疊層材料、阻劑(resist)、增建疊層板材料等,可廣泛且有效地利用,特別是,尤其可有效利用作為近年之資訊終端設備或通信設備等之因應高積體、高密度化之印刷電路板材料。此外,關於本發明之覆金屬箔疊層板等,因為具有鍍敷剝離強度優良之性能,為工業方面之實用性極高者。
Claims (8)
- 一種樹脂組成物,含有下列通式(2)表示之萘酚芳烷基型氰酸酯化合物(A)及下列通式(1)表示之環氧樹脂(B);該通式(2)表示之萘酚芳烷基型氰酸酯化合物(A)之含量相對於該樹脂組成物中之樹脂固體成分之總量100質量份為40~60質量份;該通式(1)表示之環氧樹脂(B)之含量相對於該樹脂組成物中之樹脂固體成分之總量100質量份為40~60質量份;
- 如申請專利範圍第1項之樹脂組成物,更含有填充材(C)。
- 如申請專利範圍第2項之樹脂組成物,其中,該填充材(C)之含量相對於該樹脂組成物中之樹脂固體成分之總量(100質量份)為50~1600質量份。
- 一種預浸體,具有:基材;及含浸或塗佈於該基材之如申請專利範圍第1或2項之樹脂組成物。
- 一種覆金屬箔疊層板,具有:至少重疊了1片或2片以上之如申請專利範圍第5項之預浸體;與疊層並成形在該預浸體之單面或兩面之金屬箔。
- 一種樹脂片,具有:片狀基材;與塗佈在該片狀基材之單面或兩面並進行了乾燥的如申請專利範圍第1或2項之樹脂組成物。
- 一種印刷電路板,包含:絕緣層;與形成在該絕緣層之單面或兩面之導體層;該絕緣層含有如申請專利範圍第1或2項之樹脂組成物。
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US (1) | US20180092218A1 (zh) |
EP (1) | EP3290454B1 (zh) |
JP (1) | JP6788807B2 (zh) |
KR (1) | KR102481055B1 (zh) |
CN (1) | CN107531882A (zh) |
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WO (1) | WO2016175106A1 (zh) |
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JP2006229038A (ja) * | 2005-02-18 | 2006-08-31 | Nippon Zeon Co Ltd | 多層プリント配線板の製造方法 |
JP2007227567A (ja) * | 2006-02-22 | 2007-09-06 | Nippon Zeon Co Ltd | 金属薄膜層の形成方法および多層プリント配線板の製造方法 |
JP2007284467A (ja) * | 2006-04-12 | 2007-11-01 | Yokohama Rubber Co Ltd:The | エポキシ樹脂組成物 |
JP2007284474A (ja) * | 2006-04-12 | 2007-11-01 | Yokohama Rubber Co Ltd:The | エポキシ樹脂組成物 |
WO2013008684A1 (ja) * | 2011-07-14 | 2013-01-17 | 三菱瓦斯化学株式会社 | プリント配線板用樹脂組成物 |
SG11201401958TA (en) * | 2011-11-02 | 2014-09-26 | Mitsubishi Gas Chemical Co | Resin composition, prepreg, and laminate |
CN104169343B (zh) * | 2012-03-23 | 2018-09-14 | 三菱瓦斯化学株式会社 | 预浸料和层压板 |
JP2014108531A (ja) * | 2012-11-30 | 2014-06-12 | Mitsubishi Paper Mills Ltd | 銀めっき塗装体 |
KR101741771B1 (ko) * | 2012-03-27 | 2017-05-30 | 미쓰비시 세이시 가부시키가이샤 | 은도금 도장체 |
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JP2014205755A (ja) * | 2013-04-11 | 2014-10-30 | 住友ベークライト株式会社 | プライマー層形成用樹脂組成物 |
KR102157499B1 (ko) * | 2013-06-18 | 2020-09-18 | 미츠비시 가스 가가쿠 가부시키가이샤 | 수지 조성물, 프리프레그, 수지 시트 및 금속박 피복 적층판 |
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- 2016-04-20 EP EP16786383.6A patent/EP3290454B1/en active Active
- 2016-04-20 WO PCT/JP2016/062569 patent/WO2016175106A1/ja active Application Filing
- 2016-04-20 CN CN201680024002.1A patent/CN107531882A/zh active Pending
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US3936575A (en) * | 1973-02-21 | 1976-02-03 | Sumitomo Bakelite Company, Limited | Flexible metal-clad laminates and method for manufacturing the same |
TW201348311A (zh) * | 2012-03-30 | 2013-12-01 | Mitsubishi Gas Chemical Co | 樹脂組成物、預浸體及疊層板 |
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EP3290454B1 (en) | 2020-05-06 |
EP3290454A4 (en) | 2018-09-12 |
WO2016175106A1 (ja) | 2016-11-03 |
JPWO2016175106A1 (ja) | 2018-02-22 |
CN107531882A (zh) | 2018-01-02 |
JP6788807B2 (ja) | 2020-11-25 |
KR102481055B1 (ko) | 2022-12-23 |
EP3290454A1 (en) | 2018-03-07 |
US20180092218A1 (en) | 2018-03-29 |
KR20170141701A (ko) | 2017-12-26 |
TW201704283A (zh) | 2017-02-01 |
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