TWI768081B - 印刷配線板用樹脂組成物、預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板及多層印刷配線板 - Google Patents
印刷配線板用樹脂組成物、預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板及多層印刷配線板 Download PDFInfo
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- TWI768081B TWI768081B TW107124026A TW107124026A TWI768081B TW I768081 B TWI768081 B TW I768081B TW 107124026 A TW107124026 A TW 107124026A TW 107124026 A TW107124026 A TW 107124026A TW I768081 B TWI768081 B TW I768081B
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- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
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- 229910000679 solder Inorganic materials 0.000 description 1
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- 239000004408 titanium dioxide Substances 0.000 description 1
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- MQVCTPXBBSKLFS-UHFFFAOYSA-N tri(propan-2-yloxy)-propylsilane Chemical compound CCC[Si](OC(C)C)(OC(C)C)OC(C)C MQVCTPXBBSKLFS-UHFFFAOYSA-N 0.000 description 1
- DENFJSAFJTVPJR-UHFFFAOYSA-N triethoxy(ethyl)silane Chemical compound CCO[Si](CC)(OCC)OCC DENFJSAFJTVPJR-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
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- ILWRPSCZWQJDMK-UHFFFAOYSA-N triethylazanium;chloride Chemical compound Cl.CCN(CC)CC ILWRPSCZWQJDMK-UHFFFAOYSA-N 0.000 description 1
- 125000004360 trifluorophenyl group Chemical group 0.000 description 1
- LFRDHGNFBLIJIY-UHFFFAOYSA-N trimethoxy(prop-2-enyl)silane Chemical compound CO[Si](OC)(OC)CC=C LFRDHGNFBLIJIY-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- 125000003258 trimethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])[*:1] 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
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
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- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical class [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 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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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/241—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres
- C08J5/244—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs using inorganic fibres using glass fibres
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/092—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising epoxy resins
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/04—Layered products comprising a layer of synthetic resin as impregnant, bonding, or embedding substance
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/18—Layered products comprising a layer of synthetic resin characterised by the use of special additives
- B32B27/20—Layered products comprising a layer of synthetic resin characterised by the use of special additives using fillers, pigments, thixotroping agents
-
- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
一種印刷配線板用樹脂組成物,含有: 包含下述鍵結(a)、(b)、(c)及(d)之含矽聚合物(A)、 氰酸酯化合物(B)、 環氧樹脂(D)、及 填充材料(E);
Description
本發明係關於印刷配線板用樹脂組成物、預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板、及多層印刷配線板。
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微細化。伴隨於此,對於印刷配線板所使用之半導體封裝用疊層板要求之各種特性變得越來越嚴格。
為了提高對於半導體封裝用疊層板要求之各種特性而開發各種技術,其中有人開發出於印刷配線板用樹脂樹脂組成物中使用含矽化合物的技術。例如,在專利文獻1(日本特開2014-47348號公報)及專利文獻2(日本特開2015-147869號公報)中,揭示藉由含有具有特定結構之分枝狀聚矽氧烷與熱硬化性樹脂等而得之樹脂組成物來製作預浸體的技術。 [先前技術文獻] [專利文獻]
[專利文獻1]日本特開2014-47348號公報 [專利文獻2]日本特開2015-147869號公報
[發明所欲解決之課題]
近年來,於半導體封裝用疊層板用途,對於疊層板之熱膨脹率(以下有時簡稱為"熱膨脹率")的減低及對於銅箔等金屬層的剝離強度(以下有時稱為"剝離強度"。)的要求提高。特別就剝離強度之觀點,樹脂組成物中各成分的相容性(以下有時稱為"清漆相容性"。)係重要的要素之一。即使在專利文獻1及2記載之技術中,就保持良好之熱膨脹率且提高剝離強度之觀點,仍有改善的餘地。
本發明之目的係為了解決上述課題,而提供一種印刷配線板用樹脂組成物,具有良好之清漆相容性,且可形成熱膨脹率低,對於銅箔之剝離強度優良的印刷配線板;並提供使用了該印刷配線板用樹脂組成物的預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板、及多層印刷配線板。 [解決課題之手段]
本案發明者們為了解決上述課題進行深入研究。其結果發現藉由使用具有特定結構之含矽聚合物,可達成上述課題,而完成了本發明。 <1>一種印刷配線板用樹脂組成物,含有: 包含下述鍵結(a)、(b)、(c)及(d)之含矽聚合物(A)、 氰酸酯化合物(B)、 環氧樹脂(D)、及 填充材料(E); 【化1】在鍵結(a)~(d)中,R係選自碳數1~12之經取代或未取代之1價烴基,X係表示含有環氧基之1價有機基,該含矽聚合物(A)中之全部的R及X可全部相同,亦可不同。 <2>如<1>之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之環氧當量係500~4000g/eq。 <3>如<1>或<2>之印刷配線板用樹脂組成物,其中,該鍵結(a)~(d)中的R係甲基或苯基。 <4>如<1>~<3>中任一項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之全部R中之經取代或未取代之苯基的比率係50mol%~75mol%。 <5>如<1>~<4>中任一項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之重量平均分子量係5,000~20,000。 <6>如<1>~<5>中任一項之印刷配線板用樹脂組成物,其中,相對於樹脂固體成分100質量份,該含矽聚合物(A)之含量係9~25質量份。 <7>如<1>~<6>中任一項之印刷配線板用樹脂組成物,其中,該環氧樹脂(D)具有萘結構。 <8>如<1>~<7>中任一項之印刷配線板用樹脂組成物,其中,該環氧樹脂(D)係下式(NE)表示之甲酚/萘酚酚醛清漆型環氧樹脂; 【化2】此處,m、n表示1以上的整數。 <9>如<1>~<8>中任一項之印刷配線板用樹脂組成物,其中,該氰酸酯化合物(B)係下式(CN)表示之萘酚芳烷基型氰酸酯化合物; 【化3】此處,R7
各自獨立地表示氫原子或甲基,n7
表示1以上之整數。 <10>如<1>~<9>中任一項之印刷配線板用樹脂組成物,更含有馬來醯亞胺化合物(C)。 <11>如<10>之印刷配線板用樹脂組成物,其中,相對於樹脂固體成分100質量份,該填充材料(E)之含量係100~1000質量份。 <12>如<1>~<11>中任一項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)的末端為選自R、X及烷氧基之取代基。 <13>一種預浸體,具有:基材;及含浸或塗布於該基材之如<1>~<12>中任一項之印刷配線板用樹脂組成物。 <14>一種樹脂片,具有:支持體;及配置於該支持體的表面之如<1>~<12>中任一項之印刷配線板用樹脂組成物。 <15>一種疊層板,具備數個選自於由如<13>之預浸體及如<14>之樹脂片構成之群組中之一種或二種以上之材料。 <16>一種覆金屬箔疊層板,具備:選自於由如<13>之預浸體及如<14>之樹脂片構成之群組中之一種或二種以上;及金屬箔。 <17>一種印刷配線板,具備: 絕緣層,含有如<1>~<12>中任一項之印刷配線板用樹脂組成物;及 導體層,形成於該絕緣層之表面。 <18>一種多層印刷配線板,具有由第1絕緣層與第2絕緣層構成之數個絕緣層、及由第1導體層與第2導體層構成之數個導體層; 該第1絕緣層,係以疊層了至少1片以上之選自於由如<13>之預浸體及如<14>之樹脂片構成之群組中之至少一種形成; 該第2絕緣層,係以於該第1絕緣層之單面方向疊層了至少1片以上之選自於由如<13>之預浸體及如<14>之樹脂片構成之群組中之至少一種形成; 該第1導體層係配置於該數個絕緣層的各絕緣層之間; 該第2導體層係配置於該數個絕緣層之最外層的表面。 [發明之效果]
根據本發明,可提供具有良好之清漆相容性,且能形成熱膨脹率低,對於銅箔之剝離強度優良之印刷配線板的印刷配線板用樹脂組成物;並可提供使用了該印刷配線板用樹脂組成物的預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板、及多層印刷配線板。
以下,針對用以實施本發明的形態(以下稱為「本實施形態」。)進行詳細說明。然而,本發明並不限定於此,在不脫離其要旨的範圍內可有各種變形。
《印刷配線板用樹脂組成物》 本實施形態之印刷配線板用樹脂組成物(以下有時簡稱為"樹脂組成物")含有:含下述鍵結(a)、(b)、(c)及(d)的含矽聚合物(A)、氰酸酯化合物(B)、環氧樹脂(D)、及填充材料(E)。
含矽聚合物(A)具有鍵結(a)、(b)、(c)及鍵結(d)。鍵結(a)及鍵結(d)係三價的鍵結基,可使含矽聚合物(A)成為3維結構。一般而言,由鍵結(a)及鍵結(b)之構成單元構成之含矽聚合物係與其他樹脂成分的相容性差,但若含矽聚合物含有具有“含環氧基之1價有機基”的構成單元,則會改善與其他樹脂成分的相容性。尤其是使用具有為可構成3維結構之三價的鍵結基,且係具有含環氧基之1價有機基的構成單元之鍵結(d)之含矽聚合物(A)的樹脂組成物,係清漆相容性高,且與使用了不具有鍵結(d)之含矽聚合物而得之組成物相比,在為了製作預浸體等而進行硬化時之硬化物的熱膨脹率低,在形成覆金屬箔疊層板等時也可發揮優良之剝離強度。
(含矽聚合物(A)) 含矽聚合物(A)包含鍵結(a)、(b)、(c)及(d)。
鍵結(a)~(c)中,R係碳數1~12之經取代或未取代之1價烴基,可舉例如、甲基、乙基、丙基、丁基、異丙基、異丁基、第三丁基、戊基、己基、庚基、辛基、2-乙基己基等烷基;乙烯基、烯丙基、丁烯基、戊烯基、己烯基等烯基;苯基、甲苯基、二甲苯基、萘基、聯苯基等芳基;芐基、苯乙基等芳烷基等,其中,宜為甲基或苯基。含矽聚合物(A)宜為鍵結(a)~(c)之至少一個R具有經取代或未取代之苯基,更宜為鍵結(a)具有經取代或未取代之苯基。此時,含矽聚合物(A)之全部R中經取代或未取代之苯基的比率,考慮與其他熱硬化性樹脂成分(含矽聚合物(A)以外之熱硬化性樹脂成分)之相容性的觀點,宜為50mol%~75mol%。另外,考慮兼具熱膨脹率與剝離強度之觀點,更宜為含矽聚合物(A)之全部R中之經取代或未取代之苯基的比率為70mol%~75mol%。
鍵結(c)及(d)中,X係含有環氧基之1價有機基,可舉例如2,3-環氧丙基、3,4-環氧丁基、4,5-環氧戊基、2-環氧丙氧基乙基、3-環氧丙氧基丙基、4-環氧丙氧基丁基、2-(3,4-環氧環己基)乙基、3-(3,4-環氧環己基)丙基等,其中,宜為3-環氧丙氧基丙基。 此外,含矽聚合物(A)可具有鍵結(a)~(d)以外之其他鍵結。就其他鍵結而言,可舉例如鍵結(a)~(d)中之R或X為氫原子之鍵結等。
含矽聚合物(A)之末端沒有特別之限定,可為選自上述之R、X、羥基及烷氧基的取代基,除此之外也可為氫原子、苯氧基等。考慮聚合物之保存安定性的觀點,含矽聚合物(A)之末端宜為R、X、烷氧基中之任一者。就上述烷氧基而言,可列舉甲氧基、乙氧基、丙氧基、丁氧基。
含矽聚合物(A)之環氧當量沒有特別之限定,考慮提高清漆相容性之觀點,宜為500~4000g/eq之範圍,進一步宜為1000~2500g/eq,尤其宜為1000~2000g/eq。含矽聚合物(A)之軟化點沒有特別之限定,考慮含矽聚合物(A)之分散性及獲得之印刷配線板用樹脂組成物之硬化物之機械強度的觀點,宜為40℃~120℃,更宜為50℃~100℃。含矽聚合物(A)之軟化點例如可藉由含矽聚合物(A)之分子量、構成鍵結單元(例如(a)~(d)之含有比率)等適當地調整。
含矽聚合物(A)之重量平均分子量(Mw:凝膠滲透層析(GPC)測定中聚苯乙烯換算而得),考慮樹脂組成物之低彈性化、抑制渗出(bleed out)之產生的觀點,宜為3000以上,更宜為5,000~20,000,尤其宜為6,500~16,000。此外,含矽聚合物(A)宜為無規共聚物。
含矽聚合物(A)之製造方法沒有特別之限制,可藉由公知方法製造。例如,可藉由將能以水解縮合反應形成上述鍵結(a)~(d)之有機氯矽烷、有機烷氧基矽烷、矽氧烷、或它們的部分水解縮合物予以(共)水解、縮合來獲得。
就可形成鍵結(a)之化合物(以下有時稱為"化合物(a)")而言,可舉例如甲基三甲氧基矽烷、甲基三乙氧基矽烷、甲基三異丙氧基矽烷、乙基三甲氧基矽烷、乙基三乙氧基矽烷、乙基三異丙氧基矽烷、丙基三甲氧基矽烷、丙基三乙氧基矽烷、丙基三異丙氧基矽烷、苯基三甲氧基矽烷、苯基三乙氧基矽烷、乙烯基三甲氧基矽烷、烯丙基三甲氧基矽烷等。就此等化合物的市售商品而言,可舉例如苯基三甲氧基矽烷(信越化學工業(股),製品名:KBM103)、苯基三乙氧基矽烷(信越化學工業(股),製品名:KBE-103)等。
就可形成鍵結(b)之化合物(以下有時稱為"化合物(b)")而言,可舉例如二甲基二甲氧基矽烷、二甲基二乙氧基矽烷、甲基乙基二甲氧基矽烷、二乙基二甲氧基矽烷、二乙基二乙氧基矽烷、甲基丙基二甲氧基矽烷、甲基丙基二乙氧基矽烷、二異丙基二甲氧基矽烷、苯基甲基二甲氧基矽烷、乙烯基甲基二甲氧基矽烷等。就此等化合物之市售商品而言,可舉例如二甲基二甲氧基矽烷(信越化學工業(股)、製品名:KBM-22)、二甲基二乙氧基矽烷(信越化學工業(股)、製品名:KBE-22)等。
就可形成鍵結(c)之化合物(以下有時稱為"化合物(c)")而言,可舉例如γ-環氧丙氧基丙基甲基二甲氧基矽烷、γ-環氧丙氧基丙基甲基二乙氧基矽烷、β-(3,4-環氧環己基)乙基甲基二甲氧基矽烷等。就此等化合物之市售商品而言,可舉例如γ-環氧丙氧基丙基甲基二乙氧基矽烷(信越化學工業(股)、製品名:KBE-402)、β-(3,4-環氧環己基)乙基甲基二甲氧基矽烷(信越化學工業(股)、製品名:KBM-402)等。
就可形成鍵結(d)之化合物(以下有時稱為"化合物(d)")而言,可列舉γ-環氧丙氧基丙基三甲氧基矽烷、γ-環氧丙氧基丙基三乙氧基矽烷、β-(3,4-環氧環己基)乙基三甲氧基矽烷。
含矽聚合物(A)中之鍵結(a)~(d)可大致區分為三價之鍵結基的鍵結(a)及(d),與為二價之鍵結基之鍵結(b)及(c)。設鍵結(a)及(d)為"T單元"、鍵結(b)及(c)為“D單元”時,含矽聚合物(A)中T單元及D單元各別的量,考慮與其他熱硬化性樹脂成分之相容性的觀點,相對於鍵結(a)~(d)之合計100[Simol%],宜為T單元為50以上且未達100[Simol%]且D單元超過0且為50以下[Simol%],考慮對於溶劑之溶解性、低熱膨脹性之觀點,更宜為T單元為70以上85以下[Simol%]、D單元為15以上30以下[Simol%],特別宜為T單元為80以上85以下[Simol%]、D單元為15以上20以下[Simol%]。含矽聚合物(A)例如能以任意比例使用上述之各化合物(a)~(d)以使各鍵結成為上述範圍來製備。 上述之Si莫耳%係全部Si莫耳中之比率,就Si莫耳而言,若為單體則其分子量為1莫耳,若為二聚體則其平均分子量除以2而得的數為1莫耳。 含矽聚合物(A)在不妨害本發明之效果的範圍內可具有其他鍵結。
可藉由公知方法將包含化合物(a)~(d)之原料(以下有時簡稱為"化合物(a)~(d)的混合物")予以(共)水解、縮合來合成含矽聚合物(A)。例如將化合物(a)~(d)的混合物以pH為1~7.5的水,宜為pH為2~7的水使其(共)水解。此時,可使用於水中分散有二氧化矽微粒等金屬氧化物微粒者。此外,為了調整上述之pH或促進水解,亦可使用氟化氫、鹽酸、硝酸、甲酸、乙酸、丙酸、草酸、檸檬酸、馬來酸、苯甲酸、丙二酸、戊二酸、乙醇酸、甲磺酸、甲苯磺酸等有機酸及無機酸,或使用於表面具有羧酸基或磺酸基之陽離子交換樹脂等固體酸觸媒、或酸性之水分散二氧化矽微粒等水分散金屬氧化物微粒作為觸媒。此外,亦可於水解時使將二氧化矽微粒等金屬氧化物微粒分散於水或有機溶劑中而得者共存。
在上述水解中,水之使用量相對於化合物(a)~(d)之合計100質量份,可為水20~3,000質量份之範圍,考慮保存安定性、耐擦傷性、抗裂性之觀點,可為50質量份以上150質量份以下。
可藉由於化合物(a)~(d)的混合物中滴加或加入水,或於水中滴加或加入化合物(a)~(d)的混合物來進行上述水解。此時,可使用有機溶劑,亦可使其不含有有機溶劑來進行合成。例如,若使用有機溶劑,會有藉由水解獲得之含矽聚合物(A)之GPC分析中之聚苯乙烯換算重量平均分子量變小的傾向。
就獲得含矽聚合物(A)而言,在上述水解後進行縮合反應。縮合在水解後連續地進行即可,通常,考慮抑制凝膠化的觀點,係在液溫為常溫,或於100℃以下之加熱下進行。進一步地,於80℃以上、常壓或減壓下,餾去水解所產生之醇,藉此可促進縮合。另外,為了促進縮合之目的,可添加鹼性化合物、酸性化合物、金屬螯合化合物等縮合觸媒。為了調整縮合之進行程度及濃度的目的,可在縮合步驟之前或縮合步驟中添加有機溶劑,或添加使二氧化矽微粒等金屬氧化物微粒分散於水或有機溶劑中而得者。一般而言,含矽聚合物(A)在進行縮合的同時,會高分子量化且對於水或產生之醇的溶解性降低,故就添加之有機溶劑而言,宜為可充分地溶解含矽聚合物(A),沸點為80℃以上之極性較高的有機溶劑。就如此之有機溶劑的具體例而言,可舉例如異丙醇、正丁醇、異丁醇、第三丁醇、二丙酮醇等醇類;甲基丙酮、二乙酮、甲基異丁酮、環己酮等酮類;二丙基醚、二丁基醚、苯甲醚、二烷(dioxane)、乙二醇單乙基醚、乙二醇單丁基醚、丙二醇單甲基醚、丙二醇單甲基醚乙酸酯等醚類;乙酸丙酯、乙酸丁酯、乙酸環己酯等酯類等。
本實施形態之樹脂組成物中,含矽聚合物(A)之含量沒有特別之限定,考慮清漆相容性、耐熱性、耐藥品性之觀點,相對於樹脂固體成分100質量份,宜為9~25質量份。此外,在本實施形態中,稱為「樹脂固體成分」時,若無特別指明的情況下,係指樹脂組成物中除溶劑及填充材料(E)以外之成分的總量。
(氰酸酯化合物(B)) 本實施形態之樹脂組成物包含氰酸酯化合物(B)。就氰酸酯化合物(B)而言,只要是分子內具有經至少1個氰氧基(氰酸酯基)取代而得之芳香族部分的化合物即可,沒有特別之限定。使用了氰酸酯化合物的樹脂組成物製成硬化物時,具有玻璃轉移溫度、低熱膨脹性、鍍敷密接性等優良的特性。
就氰酸酯化合物的例子而言,不限定為以下之例子,可列舉下式(1)表示者。
式(1)中,Ar1
表示苯環、萘環或2個苯環經單鍵鍵結而得者。有多個Ar1
時彼此可為相同,亦可為不同。Ra係各自獨立表示氫原子、碳數1~6烷基、碳數6~12之芳基、碳數1~4之烷氧基、碳數1~6之烷基與碳數6~12之芳基鍵結而得之基。Ra之芳香環也可具有取代基,Ar1
及Ra的取代基可選擇任意位置。p係表示鍵結於Ar1
之氰氧基的數目,各自獨立地為1~3之整數。q表示鍵結於Ar1
之Ra的數目,當Ar1
為苯環時係4-p,為萘環時係6-p,為2個苯環經單鍵鍵結而得者時係8-p。t表示平均重複數,為0~50之範圍,氰酸酯化合物可為t不相同之化合物的混合物。有多個X時係各自獨立地表示單鍵、碳數1~50之2價有機基(氫原子可取代為雜原子。)、氮數1~10之2價有機基(例如-N-R-N-(此處R表示有機基。))、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者。
式(1)之Ra中之烷基可具有直鏈或分支之鏈狀結構、及環狀結構(例如環烷基等)中之任一者。 此外,式(1)之Ra中之烷基及Ra之芳基中的氫原子可取代為氟原子、氯原子等鹵素原子、甲氧基、苯氧基等烷氧基、或氰基等。 就烷基之具體例而言,不限定為以下例,可列舉甲基、乙基、丙基、異丙基、正丁基、異丁基、第三丁基、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。 就芳基之具體例而言,不限定為以下例,可列舉苯基、二甲苯基、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、間或對甲苯基等。 就烷氧基而言,不限定為以下例,可舉例如甲氧基、乙氧基、丙氧基、異丙氧基、正丁氧基、異丁氧基、及第三丁氧基。 就上述式(1)之X中之碳數1~50之2價有機基的具體例而言,不限定為以下例,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、茀二基及苯二甲內酯二基(phthalidiyl)等。該2價有機基中之氫原子可取代為氟原子、氯原子等鹵素原子、甲氧基、苯氧基等烷氧基、氰基等。 就上述式(1)之X中之氮數1~10之2價有機基的例子而言,不限定為以下例,可列舉亞胺基、聚醯亞胺基等。
此外,就式(1)中之X之有機基而言,可舉例如為下式(2)或下式(3)表示之結構。
【化7】上述式(2)中,Ar2
表示苯四基、萘四基或聯苯四基,u為2以上時,彼此可為相同亦可為不同。Rb、Rc、Rf、及Rg係各自獨立表示氫原子、碳數1~6之烷基、碳數6~12之芳基、三氟甲基、或至少具有一個苯酚性羥基的芳基。Rd及Re係各自獨立地選自氫原子、碳數1~6之烷基、碳數6~12之芳基、碳數1~4之烷氧基、或羥基中之任一種。u表示0~5之整數,亦可為u不相同之化合物的混合物。
【化8】式(3)中,Ar3
表示苯四基、萘四基或聯苯四基,v為2以上時,彼此可為相同亦可為不同。Ri及Rj係各自獨立地表示氫原子、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、或經至少1個氰氧基取代之芳基。v表示0~5之整數,亦可為v不相同之化合物的混合物。
另外,就式(1)中之X而言,可列舉下式表示之2價的基。
就式(2)之Ar2
及式(3)之Ar3
的具體例而言,可列舉:式(2)表示之2個碳原子、或式(3)表示之2個氧原子鍵結於1,4位或1,3位的苯四基;上述2個碳原子或2個氧原子鍵結於4,4’位、2,4’位、2,2’位、2,3’位、3,3’位、或3,4’位之聯苯四基;及上述2個碳原子或2個氧原子鍵結於2,6位、1,5位、1,6位、1,8位、1,3位、1,4位、或2,7位之萘四基。 式(2)之Rb、Rc、Rd、Re、Rf及Rg以及式(3)之Ri、Rj中的烷基及芳基係與上述式(1)中者為相同含意。
就上述式(1)表示之氰氧基取代芳香族化合物之具體例而言,不限定為以下例,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-乙醯胺苯、4-氰氧基二苯甲酮、1-氰氧基-2,6-二第三丁基苯、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-第三丁基苯、1,4-二氰氧基-2,4-二甲基苯、1,4-二氰氧基-2,3,4-二甲基苯、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2,7-二氰氧基二萘、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’-二氰氧基二苯基甲烷、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、4,4-二氰氧基二苯甲酮、1,3-雙(4-氰氧基苯基)-2-丙-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’-氧基二鄰苯二甲醯亞胺、雙(N-3-氰氧基-4-甲基苯基)-4,4’-氧基二鄰苯二甲醯亞胺、雙(N-4-氰氧基苯基)-4,4’-氧基二鄰苯二甲醯亞胺、雙(N-4-氰氧基-2-甲基苯基)-4,4’-(六氟亞異丙基)二鄰苯二甲醯亞胺、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-酮及2-苯基-3,3-雙(4-氰氧基苯基)吲哚啉-2-酮。
此外,就上述式(1)表示之化合物之其他具體例而言,並不限定為以下例,可列舉苯酚酚醛清漆樹脂及甲酚酚醛清漆樹脂(藉由公知之方法,將苯酚、烷基取代之苯酚或鹵素取代之苯酚與福馬林或聚甲醛等甲醛化合物於酸性溶液中使其反應而得者)、參苯酚酚醛清漆樹脂(將羥苯甲醛與苯酚在酸性觸媒之存在下使其反應而得者)、茀酚醛清漆樹脂(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)、苯酚芳烷基樹脂、甲酚芳烷基樹脂、萘酚芳烷基樹脂及聯苯芳烷基樹脂(藉由公知之方法,將如Ar4
-(CH2
Y)2
(Ar4
表示苯基,Y表示鹵素原子。以下於此段落皆為相同含意。)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;或如Ar4
-(CH2
OR)2
表示之雙(烷氧基甲基)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;或如Ar4
-(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;或將芳香族醛類化合物、芳烷基化合物與苯酚化合物縮聚而得者)、苯酚改性二甲苯甲醛樹脂(藉由公知之方法,將二甲苯甲醛樹脂與苯酚化合物於酸性觸媒之存在下使其反應而得者)、改性萘甲醛樹脂(藉由公知之方法,將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)、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(藉由公知之方法,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)等將苯酚樹脂藉由與上述同樣之方法予以氰酸酯化者以及此等之預聚合物。
上述氰酸酯化合物可單獨使用1種,或混合2種以上來使用。
上述氰酸酯化合物之中,宜為雙酚A型氰酸酯化合物、雙酚E型氰酸酯化合物、雙酚F型氰酸酯化合物等雙酚型氰酸酯化合物、萘酚芳烷基型氰酸酯化合物、及苯酚酚醛清漆型氰酸酯化合物。亦即,在本實施形態中,氰酸酯化合物宜含有選自於由雙酚型氰酸酯化合物、萘酚芳烷基型氰酸酯化合物、及苯酚酚醛清漆型氰酸酯化合物構成之群組中之至少一種。進一步,氰酸酯化合物更宜含有萘酚芳烷基型氰酸酯化合物。
就上述萘酚芳烷基型氰酸酯化合物而言,可列舉下式(CN)表示之萘酚芳烷基型氰酸酯化合物。
氰酸酯化合物之含量可因應期望之特性適當地設定,沒有特別之限定,考慮耐熱性、耐藥品性之觀點,相對於樹脂固體成分100質量份,宜為5~60質量份,更宜為10~50質量份,進一步宜為20~30質量份。
(馬來醯亞胺化合物(C)) 本實施形態之樹脂組成物可任意地含有馬來醯亞胺化合物(C)。就馬來醯亞胺化合物(C)而言,只要是分子中具有1個以上之馬來醯亞胺基的化合物,便沒有特別之限定,可舉例如N-苯基馬來醯亞胺、N-羥基苯基馬來醯亞胺、雙(4-馬來醯亞胺苯基)甲烷、2,2-雙{4-(4-馬來醯亞胺苯氧基)-苯基}丙烷、雙(3,5-二甲基-4-馬來醯亞胺苯基)甲烷、雙(3-乙基-5-甲基-4-馬來醯亞胺苯基)甲烷、雙(3,5-二乙基-4-馬來醯亞胺苯基)甲烷、下述式(4)表示之馬來醯亞胺化合物、此等馬來醯亞胺化合物的預聚物、或馬來醯亞胺化合物與胺化合物之預聚物。此等之中,宜為選自於由2,2’-雙{4-(4-馬來醯亞胺苯氧基)-苯基}丙烷、雙(3-乙基-5-甲基-4-馬來醯亞胺苯基)甲烷及下述式(4)表示之馬來醯亞胺化合物構成之群組中之至少1種。藉由含有如此之馬來醯亞胺化合物(C),有獲得之硬化物的熱膨脹率更減低,玻璃轉移溫度更優良的傾向。考慮相同之觀點,馬來醯亞胺化合物(C)更宜含有選自於由下述式(4)表示之馬來醯亞胺化合物構成之群組中之至少1種。
此處,式(4)中,R5
係各自獨立表示氫原子或甲基,宜為氫原子。此外,式(4)中,n1
表示1以上之整數,宜為10以下之整數,更宜為7以下之整數。
本實施形態之馬來醯亞胺化合物(C)之含量相對於樹脂固體成分100質量份,宜為10~50質量份,更宜為10~30質量份,進一步宜為15~20質量份。藉由使馬來醯亞胺化合物(C)之含量為上述範圍內,有獲得之硬化物的熱膨脹率更減低,耐熱性更改善之傾向。
(環氧樹脂(D)) 本實施形態之樹脂組成物係包含環氧樹脂(D)。就環氧樹脂(D)而言,宜為1分子中具有2個以上之環氧基的環氧樹脂,可適合使用公知者。環氧樹脂(D)之種類沒有特別之限定,係與上述含矽聚合物(A)不相同者。就環氧樹脂(D)而言,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、萘醚型環氧樹脂、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、脂環族環氧樹脂、多元醇型環氧樹脂、含磷環氧樹脂、環氧丙胺、環氧丙酯、將丁二烯等之雙鍵經環氧化而得之化合物、藉由含羥基之聚矽氧樹脂類與環氧氯丙烷的反應所獲得之化合物等。此等環氧樹脂之中,就阻燃性、耐熱性方面,宜為聯苯芳烷基型環氧樹脂、萘醚型環氧樹脂、多官能苯酚型環氧樹脂、萘型環氧樹脂。此等環氧樹脂可單獨使用1種或組合2種以上來使用。
此等之中,就環氧樹脂(D)而言,考慮耐熱性、耐藥品性、熱膨脹率之觀點,宜為具有萘結構之環氧樹脂,尤其宜為下述式(NE)表示之甲酚/萘酚酚醛清漆型環氧樹脂。此外,下述(NE)表示之化合物係甲酚酚醛清漆環氧化合物之構成單元與萘酚酚醛清漆環氧化合物之構成單元的無規共聚物,末端可為甲酚環氧及萘酚環氧之任一者。
上述式(NE)中m、n係各別表示1以上之整數。關於m及n之上限及其比並沒有特別之限制,考慮熱膨脹率之觀點,m:n(惟,m+n=100)宜為30~50:70~50,尤其宜為45~55:55~45。
環氧樹脂(D)之含量可因應期望之特性適當地設定,沒有特別之限定,考慮柔軟性、銅箔剝離強度、耐藥品性及耐除膠渣性(desmear resistance)之觀點,相對於樹脂固體成分100質量份,宜為20~50質量份,更宜為25~45質量份,進一步宜為30~40質量份。
-苯酚樹脂- 就苯酚樹脂而言,只要是1分子中具有2個以上的羥基的苯酚樹脂,便可使用一般公知者。就其具體例而言,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、脂環族苯酚樹脂、多元醇型苯酚樹脂、含磷苯酚樹脂、含羥基之聚矽氧樹脂類等,但沒有特別之限定。此等苯酚樹脂之中,就阻燃性之觀點宜為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、含羥基之聚矽氧樹脂。此等苯酚樹脂可單獨使用1種或組合2種以上來使用。
-氧雜環丁烷樹脂- 就氧雜環丁烷樹脂而言,可使用一般公知者。可舉例如氧雜環丁烷、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)、OXT-121(東亞合成製商品名)等,沒有特別之限定。此等氧雜環丁烷樹脂可單獨使用1種或混合2種以上來使用。
-苯并 化合物- 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,便可使用一般公知者。可舉例如雙酚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)、雙酚S型苯并 BS-BXZ(小西化學製商品名)、P-d型苯并 (四國化成工業製商品名)、F-a型苯并 (四國化成工業製商品名)等,沒有特別之限定。此等苯并 化合物可使用1種或混合2種以上使用。
-具有可聚合之不飽和基的化合物- 就具有可聚合之不飽和基的化合物而言,可使用一般公知者。可舉例如乙烯、丙烯、苯乙烯、二乙烯基苯、二乙烯基聯苯等乙烯基化合物;(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、聚丙二醇二(甲基)丙烯酸酯、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、新戊四醇四(甲基)丙烯酸酯、二新戊四醇六(甲基)丙烯酸酯等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;及苯并環丁烯樹脂,沒有特別之限定。此等具有不飽和基的化合物可使用1種或混合2種以上使用。此外,上述「(甲基)丙烯酸酯」的含意係包括丙烯酸酯及對應其之甲基丙烯酸酯。
(填充材料(E)) 本實施形態之樹脂組成物含有填充材料(E)。就上述填充材料(E)而言,可列舉無機填充材料或有機填充材料。此等可各別單獨使用,亦可併用多種。 就填充材料(E)而言,可適當地使用公知者,其種類沒有特別之限定。尤其在疊層板用途中一般所使用之填充材料能適合用來作為填充材料(E)。 就無機填充材料之具體例而言,不限定為以下例,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、氧化鋯等氧化物;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。此等無機填充材料可單獨使用1種或組合2種以上使用。 此等之中,就無機填充材料而言,宜為選自於由二氧化矽、氫氧化鋁、水鋁石、氧化鎂及氫氧化鎂構成之群組中之1種或2種以上。藉由使用此等無機填充材料,有更改善樹脂組成物之熱膨脹特性、尺寸安定性、阻燃性等特性的傾向。
本實施形態之樹脂組成物中填充材料(E)的含量可因應期望之特性適當地設定,沒有特別之限定,考慮樹脂組成物之成形性的觀點,相對於樹脂固體成分100質量份,宜為40~1000質量份,更宜為100~1000質量份,進一步宜為100~750質量份,尤其宜為100~300質量份。此外,填充材料(E)之含量係指無機填充材料與有機填充材料之總量的含意。 本實施形態之樹脂組成物中無機填充材料的含量可因應期望之特性適當地設定,沒有特別之限定,考慮樹脂組成物之成形性的觀點,相對於樹脂固體成分100質量份,宜為40~1000質量份,更宜為100~750質量份,進一步宜為100~300質量份。
就上述有機填充材料之具體例而言,可列舉苯乙烯型、丁二烯型、丙烯酸型等橡膠粉末、核殼(core shell)型之橡膠粉末、聚矽氧樹脂粉末、聚矽氧橡膠粉末、聚矽氧複合粉末等。 若使用有機填充材料,有更改善樹脂組成物之熱膨脹率、柔軟性之賦予、阻燃性等特性的傾向。 本實施形態之樹脂組成物中有機填充材料的含量可因應期望之特性適當地設定,沒有特別之限制,考慮樹脂組成物之熱膨脹率、柔軟性之賦予、阻燃性等特性之觀點,相對於樹脂固體成分100質量份,宜為0~25質量份,更宜為10~25質量份。
本實施形態之樹脂組成物可併用填充材料(E)與矽烷偶聯劑或濕潤分散劑。就矽烷偶聯劑而言,可適當使用一般於無機物之表面處理所使用者,其種類沒有特別之限定。作為矽烷偶聯劑,具體而言,不限定為以下例,可列舉γ-胺基丙基三乙氧基矽烷、N-β-(胺基乙基)-γ-胺基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-環氧環己基)乙基三甲氧基矽烷等環氧矽烷系;γ-甲基丙烯醯氧基丙基三甲氧基矽烷、乙烯基-三(β-甲氧基乙氧基)矽烷等乙烯基矽烷系;N-β-(N-乙烯基苄基胺乙基)-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,可適當使用一般塗料用所使用者,其種類沒有特別之限定。宜使用共聚合系之濕潤分散劑來作為濕潤分散劑,可為市售商品。就市售商品之具體例而言可列舉BYK Japan(股)製的Disperbyk-110、111、161、180、BYK-W996、BYK-W9010、BYK-W903、BYK-W940等。濕潤分散劑可單獨使用1種或組合2種以上使用。
(硬化促進劑) 此外,本實施形態之樹脂組成物可含有用以適當地調節硬化速度的硬化促進劑。就該硬化促進劑而言,可適當地使用一般使用來作為氰酸酯化合物或環氧樹脂等的硬化促進劑者,其種類沒有特別之限定。就硬化促進劑之具體例而言,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、二甲苯酚、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、苄基二甲胺、4-甲基-N,N-二甲基苄胺等胺類;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、或偶氮雙異丁腈等偶氮化合物、N,N-二甲基胺基吡啶。硬化促進劑可單獨使用1種或組合2種以上使用。
(其它添加劑) 另外,本實施形態之樹脂組成物在不損害期望之特性的範圍內,可併用其他熱硬化性樹脂、熱塑性樹脂及其寡聚物、彈性體類等各種高分子化合物、阻燃性化合物、以及各種添加劑等。此等只要是一般所使用者便沒有特別之限定。就阻燃性化合物之具體例而言,不限定為以下者,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、三聚氰胺及苯胍胺等氮化合物、含 環之化合物、及聚矽氧系化合物等。此外,就各種添加劑而言,不限定為以下例,可舉例如紫外線吸収劑、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。此等因應期望可單獨使用1種或組合2種以上來使用。
(有機溶劑) 此外,本實施形態之樹脂組成物,因應需求可含有有機溶劑。此時,本實施形態之樹脂組成物能以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與有機溶劑互溶之態樣(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溶解或可互溶者即可,宜為可全部溶解或互溶者,可適當地使用公知者,其種類沒有特別之限制。就有機溶劑之具體例而言,可列舉丙酮、甲乙酮、甲基異丁酮等酮類;丙二醇單甲醚、丙二醇單甲醚乙酸酯等賽珞蘇(cellosolve)系溶劑;乳酸甲酯、乙酸甲酯、乙酸乙酯、乙酸丁酯、乙酸異戊酯、乳酸乙酯、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。
本實施形態之樹脂組成物可依循通常方法來製備,只要是可獲得均勻地含有本實施形態中之含矽聚合物(A)、氰酸酯化合物(B)、環氧樹脂(D)、填充材料(E)及上述之其他任意成分的樹脂組成物的方法即可,其製備方法沒有特別之限制。例如,藉由將本實施形態中之各成分依序摻合至溶劑中,充分地攪拌而可輕易地製備本實施形態之樹脂組成物。
此外,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,在均勻分散填充材料(E)時,藉由使用附設有具適當攪拌能力之攪拌機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可用來作為預浸體、樹脂片、疊層板、覆金屬箔疊層板、印刷配線板、及多層印刷配線板、或半導體封裝之構成材料。例如,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,可獲得預浸體。 此外,使用可剝離之塑膠薄膜作為基材,藉由將使本實施形態之樹脂組成物溶解於溶劑而得之溶液塗布於該塑膠薄膜並進行乾燥,可獲得增建(build-up)用薄膜或乾膜阻焊膜。此處,溶劑可於20℃~150℃之溫度乾燥1~90分鐘來進行乾燥。 此外,本實施形態之樹脂組成物可於只乾燥溶劑之未硬化之狀態使用,也可因應需求使其成為半硬化(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樹脂組成物。本實施形態之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,便沒有特別之限定。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℃之乾燥機中乾燥約2~15分鐘之方法等使其半硬化,可製造本實施形態之預浸體。此時,樹脂組成物對於基材之附著量,也就是樹脂組成物的含量(包含填充材料(E)。)相對於半硬化後之預浸體之總量宜為20~99質量%之範圍。
就製造本實施形態之預浸體時所使用之基材而言,可為各種印刷配線板材料中所使用之公知者。就如此之基材而言,可舉例如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,但沒有特別限定為此等。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種或適當地組合2種以上使用。織布之中,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,經環氧矽烷處理、胺基矽烷處理等以矽烷偶聯劑等進行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。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。
《樹脂片》 本實施形態之樹脂片係指支持體與配置於該支持體之表面的上述樹脂組成物層(疊層片),或也單指除去支持體後的樹脂組成物層(單層片)。亦即,本實施形態之樹脂片係至少具有本實施形態之樹脂組成物。該疊層片可藉由將使上述樹脂組成物溶解於溶劑而得之溶液塗布於支持體並進行乾燥來獲得。就此處使用之支持體而言,沒有特別之限定,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薄膜、乙烯四氟乙烯共聚合物薄膜、及於此等薄膜的表面塗布了脫模劑之脫模薄膜、聚醯亞胺薄膜等有機系之薄膜基材;銅箔、鋁箔等導體箔;玻璃板、SUS板、FRP等板狀之無機系之薄膜。就塗布方法而言,可舉例如將上述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式塗抹器等塗布於支持體上,而製作支持體與樹脂組成物層成為一體的疊層片之方法。此外,藉由從塗布後更進行乾燥而獲得之樹脂片,將支持體剝離或蝕刻,也可獲得單層片。此外,藉由將使上述本實施形態之樹脂組成物溶解於溶劑或與溶劑互溶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。
此外,本實施形態之樹脂片或單層片之製造中,除去溶劑時的乾燥條件沒有特別之限定,宜於20℃~200℃之溫度乾燥1~90分鐘。若為20℃以上,可更防止溶劑殘留於樹脂組成物中,若為200℃以下可抑制樹脂組成物之硬化的進展。此外,本實施形態之樹脂片或單層片中樹脂層的厚度可藉由本實施形態之樹脂組成物之溶液的濃度與塗布厚度來調整,沒有特別之限定。惟,其厚度宜為0.1~500μm。若樹脂層之厚度為500μm以下,則在乾燥時溶劑更不易殘留。 上述預浸體及樹脂片係可用來作為具備多個選自此等預浸體及樹脂片之群組中之一種或二種以上之材料的疊層板。
《覆金屬箔疊層板》 本實施形態之覆金屬箔疊層板係具有疊層至少1片以上之上述預浸體或樹脂片,及配置在該預浸體或樹脂片之單面或兩面的金屬箔。具體而言,可藉由對於1片上述預浸體或樹脂片,或重疊數片預浸體或樹脂片而得者,在其單面或兩面配置銅或鋁等金屬箔,並進行疊層成形來製作。此處使用之金屬箔,只要是印刷配線板材料中所使用者,便沒有特別之限定,宜為壓延銅箔或電解銅箔等銅箔。此外,金屬箔之厚度沒有特別之限定,宜為1~70μm,更宜為1.5~35μm。就成形條件而言,可採用通常印刷配線板用疊層板及多層板之製作中使用的方法。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、面壓20~100kg/cm2
之條件進行疊層成形,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配線板組合且疊層成形,也可製作多層板。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,以上述條件疊層成形後,形成內層電路,對該電路實施黑化處理而形成內層電路板。進一步將此內層電路板與上述之預浸體交替地各1片逐一配置,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成形。能以如此方式製作多層板。
《印刷配線板》 本實施形態之覆金屬箔疊層板藉由進一步地形成圖案,可適合用來作為印刷配線板。印刷配線板可依循通常方法進行製造,其製造方法沒有特別之限定。以下展示印刷配線板之製造方法的一例。首先準備上述之覆金屬箔疊層板。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黏接強度的表面處理,接著於該內層電路表面重疊所需片數之上述預浸體。更於其外側疊層外層電路用的金屬箔,經加熱加壓而成形為一體。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,進一步地藉由對外層電路用之金屬箔施以蝕刻處理形成外層電路,以製造印刷配線板。
藉由上述製造例獲得之印刷配線板為以下之構成:具有絕緣層;與形成在該絕緣層表面之導體層;絕緣層含有上述之本實施形態之樹脂組成物。亦即,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的層(由本實施形態之樹脂組成物構成之層)係由含有本實施形態之樹脂組成物的絕緣層所構成。
《多層印刷配線板》 如上述,本實施形態之印刷配線板適宜為具有由第1絕緣層及第2絕緣層構成之多個絕緣層與由第1導體層及第2導體層構成之多個導體層之態樣,該第1絕緣層係以疊層了至少1片以上之選自於由上述的預浸體及樹脂片之群組中之至少1種形成,該第2絕緣層係以於該第1絕緣層之單面方向疊層了至少一片以上之選自於由上述預浸體及樹脂片構成之群組中之至少1種形成,該第1導體層係配置於該多個絕緣層的各絕緣層之間中,該第2導體層係配置於該多個絕緣層之最外層的表面。根據本發明者們所知,通常的疊層板係於一芯基板的兩面方向疊層另外的預浸體而得的多層印刷配線板,而本實施形態之預浸體,可適合使用於僅在形成第1絕緣層之一預浸體的單面方向,疊層形成第2絕緣層之另外的預浸體而得的無芯型多層印刷配線板(多層無芯基板)的製造中。此外,如此之多層印刷配線板,例如可為於1層之第1絕緣層疊層2層第2絕緣層而成之構成(亦即,多個絕緣層為3層的構成)。第1導體層及第2絶緣層各別可為1層,亦可為2層以上。 [實施例]
以下,藉由使用實施例及比較例來更具體地說明本發明。本發明不因以下的實施例而有任何限定。
[合成例1]聚矽倍半氧烷(含矽聚合物)之合成 如下述方式進行聚矽倍半氧烷1~4(PO1~4)的合成。依循下述表1之記載,於2L燒瓶中加入苯基三甲氧基矽烷(下述單元結構A)、二甲基二甲氧基矽烷(下述單元結構B)、γ-環氧丙氧基丙基甲基二甲氧基矽烷(下述單元結構C)、γ-環氧丙氧基丙基三甲氧基矽烷(下述單元結構D),使液溫冷卻為約10℃。冷却後,滴加SNOWTEX(日產化學工業(股)製:水分散二氧化矽微粒、平均粒徑15~20nm、含有SiO2
20質量%之產品)211g、0.25N之乙酸水溶液93g,使內溫不超過40℃邊進行冷卻邊進行水解。滴加結束後,於40℃以下攪拌1小時,然後於60℃攪拌3小時,完成水解。 之後,投入環己酮300g,於常壓使液溫加熱至92℃來餾去水解所產生之甲醇,同時使其縮合,之後加入作為稀釋劑之異丙醇400g、塗平劑(信越化學工業(株)製:KP-341)0.5g、乙酸1.6g、及25質量%四甲基氫氧化銨(TMAH)水溶液1.6g,經攪拌後,進行濾紙過濾,獲得無色透明之聚矽倍半氧烷的溶液。此外,針對各聚矽倍半氧烷,藉由標準聚苯乙烯作為基準之GPC分析而得的重量平均分子量表示於表1。此外,在表1中表示用來作為比較用之聚矽倍半氧烷AY-42-119的組成。
[合成例2]α-萘酚芳烷基型氰酸酯樹脂(SN495VCN)之合成 將α-萘酚芳烷基樹脂(SN495V、OH基當量:236g/eq.、新日鐵化學(股)製:包含萘酚芳烷基之重複單元數n為1~5者。)0.47莫耳(OH基換算)溶解於氯仿500ml,添加三乙胺0.7莫耳至該溶液中,製備溶液1。在將溫度保持在-10℃的情況下,將該溶液1花費1.5小時滴加至0.93莫耳的氯化氰之氯仿溶液300g中,滴加結束後,攪拌30分鐘。之後,更對於獲得之溶液滴加0.1莫耳之三乙胺與氯仿30g的混合溶液,攪拌30分鐘完成反應。將副產生之三乙胺之鹽酸鹽從反應液過濾分離後,將獲得之濾液以0.1N鹽酸500ml清洗後,以水500ml進行清洗,此清洗重複進行4次。將其藉由硫酸鈉乾燥後,於75℃蒸發,更藉由於90℃進行減壓脱氣,獲得褐色固體之上述式(2)表示(式中的R7
皆為氫原子,n=1~5)α-萘酚芳烷基型氰酸酯化合物。將獲得之α-萘酚芳烷基型氰酸酯化合物藉由紅外線吸收光譜進行分析時,確認到於2264cm-1
附近之氰酸酯基的吸收。
[實施例1] 將下述組成進行混合,以甲乙酮進行稀釋,獲得清漆。 [組成] ・合成例1獲得之聚矽倍半氧烷2(PO2)10質量份 ・合成例2獲得之α-萘酚芳烷基型氰酸酯樹脂(SN495VCN)30質量份 ・酚醛清漆馬來醯亞胺(大和化成工業公司製、製品名:BMI-2300)20質量份 ・甲酚/萘酚酚醛清漆環氧化合物(DIC(股)製、製品名:HP-9540,環氧當量:242g/eq.)40質量份 ・漿液二氧化矽(Admatechs製、製品名:SC-2050MB)140質量份 ・漿液二氧化矽(Admatechs製、製品名:SC-5050MOB)60質量份 ・聚矽氧複合粉末(信越化學工業(股)製、製品名:KMP-600)25質量份 ・矽烷偶聯劑(信越化學工業(股)製、製品名:KBM-403)5.0質量份 ・濕潤分散劑(BYK JAPAN(股)製、製品名:disperbyk-161)1質量份 ・濕潤分散劑(BYK JAPAN(股)製、製品名:BYK-111)1質量份 ・三苯基咪唑(TPIZ:2,4,5-Triphenylimidazole,東京化成工業(股)製)0.5質量份 ・辛酸錳(OCt-Mn(聚合觸媒):日本化學產業(股)製、製品名:NIKKA OCTHIX Manganese)0.05質量份
[實施例2] 使用聚矽倍半氧烷2(PO2)15質量份、α-萘酚芳烷型氰酸酯樹脂28質量份、酚醛清漆馬來醯亞胺19質量份、甲酚/萘酚酚醛清漆環氧化合物38質量份,除此以外,以與實施例1同樣之方式獲得清漆。
[實施例3] 使用聚矽倍半氧烷2(PO2)20質量份、α-萘酚芳烷型氰酸酯樹脂27質量份、酚醛清漆馬來醯亞胺18質量份、甲酚/萘酚酚醛清漆環氧化合物35質量份,除此以外,以與實施例1同樣之方式獲得清漆。
[實施例4] 使用聚矽倍半氧烷2(PO2)25質量份、α-萘酚芳烷型氰酸酯樹脂25質量份、酚醛清漆馬來醯亞胺17質量份、甲酚/萘酚酚醛清漆環氧化合物33質量份,除此以外,以與實施例1同樣之方式獲得清漆。
[實施例5] 使用聚矽倍半氧烷1(PO1)15質量份來替代聚矽倍半氧烷2(PO2),除此以外,以與實施例2同樣之方式獲得清漆。
[實施例6] 使用聚矽倍半氧烷3(PO3)15質量份來替代聚矽倍半氧烷2(PO2),除此以外,以與實施例2同樣的方式獲得清漆。
[比較例1] 不使用聚矽倍半氧烷2(PO2),使用α-萘酚芳烷型氰酸酯樹脂33質量份、酚醛清漆馬來醯亞胺22質量份、甲酚/萘酚酚醛清漆環氧45質量份,除此以外,以與實施例1同樣的方式獲得清漆。
[比較例2] 使用AY42-119(聚矽倍半氧烷(環氧改性):Dow Corning Toray Co.,Ltd.製)15質量份來替代聚矽倍半氧烷2(PO2),除此以外,以與實施例2同樣之方式獲得清漆。
[比較例3] 使用聚矽倍半氧烷4(PO4)15質量份來替代聚矽倍半氧烷2(PO2),除此以外,以與實施例2同樣之方法獲得清漆。
[比較例4] 使用末端胺基改性聚矽氧(信越化學工業(股),製品名:X-22-161B)15質量份來替代聚矽倍半氧烷2(PO2),除此以外,以與實施例2同樣之方式獲得清漆。
[覆銅疊層板的製造] 將獲得之清漆含浸塗佈於厚度0.05mm之E玻璃布,使用乾燥機(耐壓防爆型蒸氣乾燥機、高杉製作所(股)製))於165℃加熱乾燥4分鐘,獲得樹脂含量73vol%的預浸體。重疊2片該預浸體,於兩面配置12μm銅箔(3EC-M3-VLP、三井金屬礦業(股)製),以壓力40kg/cm2
、溫度220℃進行80分鐘真空加壓,獲得厚度0.16mm之12μm覆銅疊層板。
(清漆互溶性) 藉由100mL之玻璃試管,將獲得之清漆於常溫(25℃)保存24小時。保存後,藉由目視觀察玻璃試管內之液體界面的分離狀態,依循以下基準評價清漆相容性。 [基準] A:未確認到成分的分離。 C:有確認到成分的分離(形成了源自聚矽氧成分之無色透明的界面)。
(熱膨脹率) 對於獲得之覆銅疊層板,針對疊層板之絕緣層,藉由JlS C 6481所規定之TMA法(Thermo-mechanical analysis)測定玻璃布之縱方向的熱膨脹係數,求得該熱膨脹係數值。具體而言,藉由蝕刻除去上述獲得之覆銅疊層板之兩面的銅箔後,以熱機械分析裝置(TA Instruments.製)從40℃至340℃以每分鐘10℃進行升溫,測定從60℃至120℃的線熱膨脹係數(ppm/℃)。進行5次同樣的測定,求出平均值(n=5之平均値)作為"熱膨脹率"並表示於下述表3。
(銅箔剝離強度) 銅箔剝離強度:針對獲得之覆銅疊層板,依循JIS C6481,使用12μm覆金屬箔的試驗片(30mm×150mm×0.8mm),以試驗數3測定銅箔之剝離強度,將下限値的平均値作為測定値。表示將比較例1之測定値設為100時的相對值(相對於比較例1的百分比)。 【表3】
從表3可知,使用了包含鍵結(d)之含矽聚合物之實施例的清漆係互溶性優良,與未使用含矽聚合物之比較例1相比,抑制銅箔剝離強度的減低,展示80%以上之優良的剝離強度。此外,可知與比較例1相比,係熱膨脹率較低。另一方面,使用了不含有鍵結(d)之含矽聚合物的比較例2及3,熱膨脹率較高一些,且剝離強度未達80%,比實施例差。此外,使用了末端胺基改性聚矽氧的比較例4係清漆互溶性差且發生滲出,無法形成塗布膜。 [產業上利用性]
本發明之樹脂組成物係作為預浸體、覆金屬箔疊層板、樹脂片、印刷配線板等之材料,具有產業上利用性。
2017年7月11日提申之日本國專利申請2017-135285號揭示之全部內容皆納入本說明書作為參照。 此外,於本說明書中所記載之全部文獻、專利申請及技術規格係與具體且個別記載各個文獻、專利申請及技術規格時為相等程度地納入本說明書中作為參照。
Claims (18)
- 如申請專利範圍第1項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之環氧當量係500~4000g/eq。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,該鍵結(a)~(d)中的R係甲基或苯基。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之全部R中之經取代或未取代之苯基的比率係50mol%~75mol%。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)之重量平均分子量係5,000~20,000。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,相對於樹脂固體成分100質量份,該含矽聚合物(A)之含量係9~25質量份。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,該環氧樹脂(D)具有萘結構。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,更含有馬來醯亞胺化合物(C)。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,相對於樹脂固體成分100質量份,該填充材料(E)之含量係100~1000質量份。
- 如申請專利範圍第1或2項之印刷配線板用樹脂組成物,其中,該含矽聚合物(A)的末端為選自R、X及烷氧基之取代基。
- 一種預浸體,具有:基材;及含浸或塗布於該基材之如申請專利範圍第1至12項中任一項之印刷配線板用樹脂組成物。
- 一種樹脂片,具有:支持體;及 配置於該支持體的表面之如申請專利範圍第1至12項中任一項之印刷配線板用樹脂組成物。
- 一種疊層板,具備數個選自於由如申請專利範圍第13項之預浸體及如申請專利範圍第14項之樹脂片構成之群組中之一種或二種以上之材料。
- 一種覆金屬箔疊層板,具備:選自於由如申請專利範圍第13項之預浸體及如申請專利範圍第14項之樹脂片構成之群組中之一種或二種以上;及金屬箔。
- 一種印刷配線板,具備:絕緣層,含有如申請專利範圍第1至12項中任一項之印刷配線板用樹脂組成物;及導體層,形成於該絕緣層之表面。
- 一種多層印刷配線板,具有由第1絕緣層與第2絕緣層構成之數個絕緣層、及由第1導體層與第2導體層構成之數個導體層;該第1絕緣層,係以疊層了至少1片以上之選自於由如申請專利範圍第13項之預浸體及如申請專利範圍第14項之樹脂片構成之群組中之至少一種形成;該第2絕緣層,係以於該第1絕緣層之單面方向疊層了至少1片以上之選自於由如申請專利範圍第13項之預浸體及如申請專利範圍第14項之樹脂片構成之群組中之至少一種形成;該第1導體層係配置於該數個絕緣層的各絕緣層之間; 該第2導體層係配置於該數個絕緣層之最外層的表面。
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