JP7409473B2 - 樹脂組成物 - Google Patents
樹脂組成物 Download PDFInfo
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- JP7409473B2 JP7409473B2 JP2022210758A JP2022210758A JP7409473B2 JP 7409473 B2 JP7409473 B2 JP 7409473B2 JP 2022210758 A JP2022210758 A JP 2022210758A JP 2022210758 A JP2022210758 A JP 2022210758A JP 7409473 B2 JP7409473 B2 JP 7409473B2
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- XDHRVAHAGMMFMC-UHFFFAOYSA-N tris(2,4-dimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC=C1P(C=1C(=CC(C)=CC=1)C)C1=CC=C(C)C=C1C XDHRVAHAGMMFMC-UHFFFAOYSA-N 0.000 description 1
- KAAYGTMPJQOOGY-UHFFFAOYSA-N tris(2,5-dimethylphenyl)phosphane Chemical compound CC1=CC=C(C)C(P(C=2C(=CC=C(C)C=2)C)C=2C(=CC=C(C)C=2)C)=C1 KAAYGTMPJQOOGY-UHFFFAOYSA-N 0.000 description 1
- RERMPCBBVZEPBS-UHFFFAOYSA-N tris(2,6-dimethylphenyl)phosphane Chemical compound CC1=CC=CC(C)=C1P(C=1C(=CC=CC=1C)C)C1=C(C)C=CC=C1C RERMPCBBVZEPBS-UHFFFAOYSA-N 0.000 description 1
- IIOSDXGZLBPOHD-UHFFFAOYSA-N tris(2-methoxyphenyl)phosphane Chemical compound COC1=CC=CC=C1P(C=1C(=CC=CC=1)OC)C1=CC=CC=C1OC IIOSDXGZLBPOHD-UHFFFAOYSA-N 0.000 description 1
- COIOYMYWGDAQPM-UHFFFAOYSA-N tris(2-methylphenyl)phosphane Chemical compound CC1=CC=CC=C1P(C=1C(=CC=CC=1)C)C1=CC=CC=C1C COIOYMYWGDAQPM-UHFFFAOYSA-N 0.000 description 1
- XRALRSQLQXKXKP-UHFFFAOYSA-N tris(3,5-dimethylphenyl)phosphane Chemical compound CC1=CC(C)=CC(P(C=2C=C(C)C=C(C)C=2)C=2C=C(C)C=C(C)C=2)=C1 XRALRSQLQXKXKP-UHFFFAOYSA-N 0.000 description 1
- LFNXCUNDYSYVJY-UHFFFAOYSA-N tris(3-methylphenyl)phosphane Chemical compound CC1=CC=CC(P(C=2C=C(C)C=CC=2)C=2C=C(C)C=CC=2)=C1 LFNXCUNDYSYVJY-UHFFFAOYSA-N 0.000 description 1
- RYXYUARTMQUYKV-UHFFFAOYSA-N tris(4-butylphenyl)phosphane Chemical compound C1=CC(CCCC)=CC=C1P(C=1C=CC(CCCC)=CC=1)C1=CC=C(CCCC)C=C1 RYXYUARTMQUYKV-UHFFFAOYSA-N 0.000 description 1
- SPNVODOGUAUMCA-UHFFFAOYSA-N tris(4-ethoxy-2,6-dimethylphenyl)phosphane Chemical compound CC1=CC(OCC)=CC(C)=C1P(C=1C(=CC(OCC)=CC=1C)C)C1=C(C)C=C(OCC)C=C1C SPNVODOGUAUMCA-UHFFFAOYSA-N 0.000 description 1
- LQEKTSMTEYLBLJ-UHFFFAOYSA-N tris(4-ethoxyphenyl)phosphane Chemical compound C1=CC(OCC)=CC=C1P(C=1C=CC(OCC)=CC=1)C1=CC=C(OCC)C=C1 LQEKTSMTEYLBLJ-UHFFFAOYSA-N 0.000 description 1
- PCCAGZSOGFNURV-UHFFFAOYSA-N tris(4-ethylphenyl)phosphane Chemical compound C1=CC(CC)=CC=C1P(C=1C=CC(CC)=CC=1)C1=CC=C(CC)C=C1 PCCAGZSOGFNURV-UHFFFAOYSA-N 0.000 description 1
- UYUUAUOYLFIRJG-UHFFFAOYSA-N tris(4-methoxyphenyl)phosphane Chemical compound C1=CC(OC)=CC=C1P(C=1C=CC(OC)=CC=1)C1=CC=C(OC)C=C1 UYUUAUOYLFIRJG-UHFFFAOYSA-N 0.000 description 1
- WXAZIUYTQHYBFW-UHFFFAOYSA-N tris(4-methylphenyl)phosphane Chemical compound C1=CC(C)=CC=C1P(C=1C=CC(C)=CC=1)C1=CC=C(C)C=C1 WXAZIUYTQHYBFW-UHFFFAOYSA-N 0.000 description 1
- NTUMNRFLAZXNBW-UHFFFAOYSA-N tris(4-propan-2-ylphenyl)phosphane Chemical compound C1=CC(C(C)C)=CC=C1P(C=1C=CC(=CC=1)C(C)C)C1=CC=C(C(C)C)C=C1 NTUMNRFLAZXNBW-UHFFFAOYSA-N 0.000 description 1
- JTOQWGJGVSYTTN-UHFFFAOYSA-N tris(4-propylphenyl)phosphane Chemical compound C1=CC(CCC)=CC=C1P(C=1C=CC(CCC)=CC=1)C1=CC=C(CCC)C=C1 JTOQWGJGVSYTTN-UHFFFAOYSA-N 0.000 description 1
- UQHFPPSBVOIUFM-UHFFFAOYSA-N tris(4-tert-butylphenyl)phosphane Chemical compound C1=CC(C(C)(C)C)=CC=C1P(C=1C=CC(=CC=1)C(C)(C)C)C1=CC=C(C(C)(C)C)C=C1 UQHFPPSBVOIUFM-UHFFFAOYSA-N 0.000 description 1
- UGNAOCDIZFIEQK-UHFFFAOYSA-N tris[4-[(2-methylpropan-2-yl)oxy]phenyl]phosphane Chemical compound C1=CC(OC(C)(C)C)=CC=C1P(C=1C=CC(OC(C)(C)C)=CC=1)C1=CC=C(OC(C)(C)C)C=C1 UGNAOCDIZFIEQK-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 239000003981 vehicle Substances 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
- 229910000166 zirconium phosphate Inorganic materials 0.000 description 1
- LEHFSLREWWMLPU-UHFFFAOYSA-B zirconium(4+);tetraphosphate Chemical compound [Zr+4].[Zr+4].[Zr+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LEHFSLREWWMLPU-UHFFFAOYSA-B 0.000 description 1
Classifications
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08L79/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4246—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof polymers with carboxylic terminal groups
- C08G59/4269—Macromolecular compounds obtained by reactions other than those involving unsaturated carbon-to-carbon bindings
- C08G59/4276—Polyesters
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- C08G64/00—Macromolecular compounds obtained by reactions forming a carbonic ester link in the main chain of the macromolecule
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- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C08G73/1046—Polyimides containing oxygen in the form of ether bonds in the main chain
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- C08G73/1053—Polyimides containing oxygen in the form of ether bonds in the main chain with oxygen only in the tetracarboxylic moiety
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- C08G73/1067—Wholly aromatic polyimides, i.e. having both tetracarboxylic and diamino moieties aromatically bound
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- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/445—Block-or graft-polymers containing polysiloxane sequences containing polyester sequences
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
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- C08L83/10—Block- or graft-copolymers containing polysiloxane sequences
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/0353—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement
- H05K1/0373—Organic insulating material consisting of two or more materials, e.g. two or more polymers, polymer + filler, + reinforcement containing additives, e.g. fillers
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- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
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Description
[1] (A)ポリイミド樹脂、及び(B)シロキサン含有ポリカーボネート樹脂を含む樹脂組成物。
[2] (A)成分の重量平均分子量が、1,000以上100,000以下である、上記[1]に記載の樹脂組成物。
[3] (B)成分が、ポリカーボネート構造を有するポリカーボネートブロックと、ポリシロキサン構造を有するポリシロキサンブロックと、を含むポリカーボネート-ポリシロキサン共重合体である、上記[1]又は[2]に記載の樹脂組成物。
[4] ポリシロキサン構造が、ポリジアルキルシロキサン構造である、上記[3]に記載の樹脂組成物。
[5] ポリカーボネート構造が、芳香族ポリカーボネート構造である、上記[3]又は[4]に記載の樹脂組成物。
[6] (B)成分中のポリシロキサン構造の含有量が、(B)成分を100質量%とした場合、1質量%以上30質量%以下である、上記[3]~[5]の何れかに記載の樹脂組成物。
[7] (B)成分の粘度平均分子量が、13,000以上25,000以下である、上記[1]~[6]の何れかに記載の樹脂組成物。
[8] (A)成分と(B)成分の質量比((A)成分/(B)成分)が、1以上5以下である、上記[1]~[7]の何れかに記載の樹脂組成物。
[9] さらに(C)無機充填材を含む、上記[1]~[8]の何れかに記載の樹脂組成物。
[10] (C)成分が、シリカである、上記[9]に記載の樹脂組成物。
[11] (C)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、30質量%以上60質量%以下である、上記[9]又は[10]に記載の樹脂組成物。
[12] さらに(D)エポキシ樹脂及び(E)硬化剤を含む、上記[1]~[11]の何れかに記載の樹脂組成物。
[13] (E)成分が、活性エステル系硬化剤を含む、上記[12]に記載の樹脂組成物。
[14] 多層フレキシブル基板の絶縁層形成用である、上記[1]~[13]の何れかに記載の樹脂組成物。
[15] 上記[1]~[14]の何れかに記載の樹脂組成物の硬化物。
[16] 支持体と、当該支持体上に設けられた上記[1]~[14]の何れかに記載の樹脂組成物で形成された樹脂組成物層とを含む、樹脂シート。
[17] 上記[1]~[14]の何れかに記載の樹脂組成物を硬化して形成される絶縁層を含む多層フレキシブル基板。
[18] 上記[17]に記載の多層フレキシブル基板を備える、半導体装置。
本発明の樹脂組成物は、(A)ポリイミド樹脂、及び(B)シロキサン含有ポリカーボネート樹脂を含む。このような樹脂組成物を用いることにより、熱膨張率が低く且つ反りが抑制された硬化物を得ることができる。また、各成分の相溶性にも優れ得る。
本発明の樹脂組成物は、(A)ポリイミド樹脂を含む。(A)ポリイミド樹脂は、繰り返し単位中にイミド結合を持つ樹脂である。(A)ポリイミド樹脂は、一般に、ジアミン化合物とテトラカルボン酸無水物とのイミド化反応により得られる樹脂を含み得る。(A)ポリイミド樹脂には、シロキサン変性ポリイミド樹脂などの変性ポリイミド樹脂も含まれる。
等が挙げられる。
本発明の樹脂組成物は、(B)シロキサン含有ポリカーボネート樹脂を含む。(B)シロキサン含有ポリカーボネート樹脂とは、主鎖又は側鎖中にポリシロキサン構造(好ましくはポリジオルガノシロキサン構造)及び主鎖の繰返し単位中に炭酸エステル結合(-O-CO-O-)を有する重合体を意味し、主鎖は、枝分れ構造を有していてもよい。(B)シロキサン含有ポリカーボネート樹脂は、例えば、ジヒドロキシ化合物をポリ炭酸エステル化して得られる、ポリカーボネート構造を有するポリカーボネートブロックと、ポリシロキサン構造(好ましくはポリジオルガノシロキサン構造)を有するポリシロキサンブロックと、を含むポリカーボネート-ポリシロキサン共重合体であり得る。
本発明の樹脂組成物は、任意の成分として(C)無機充填材を含む場合がある。(C)無機充填材は、粒子の状態で樹脂組成物に含まれる。
本発明の樹脂組成物は、任意の成分として(D)エポキシ樹脂を含む場合がある。(D)エポキシ樹脂とは、エポキシ基を有する樹脂を意味する。
本発明の樹脂組成物は、(D)エポキシ樹脂を含む場合、(D)エポキシ樹脂を硬化する機能を有する(E)硬化剤を含み得る。
本発明の樹脂組成物は、(D)エポキシ樹脂を含む場合、任意成分として、(D)エポキシ樹脂の硬化を促進させる機能を有する(F)硬化促進剤を含む場合がある。
本発明の樹脂組成物は、不揮発性成分として、さらに任意の添加剤を含んでいてもよい。このような添加剤としては、例えば、ゴム粒子、ポリアミド微粒子、シリコーン粒子等の有機充填材;(B)成分以外のポリカーボネート樹脂、フェノキシ樹脂、ポリビニルアセタール樹脂、ポリオレフィン樹脂、ポリスルホン樹脂、ポリエーテルスルホン樹脂、ポリフェニレンエーテル樹脂、ポリエーテルエーテルケトン樹脂、ポリエステル樹脂等の熱可塑性樹脂;有機銅化合物、有機亜鉛化合物、有機コバルト化合物等の有機金属化合物;フタロシアニンブルー、フタロシアニングリーン、アイオディングリーン、ジアゾイエロー、クリスタルバイオレット、酸化チタン、カーボンブラック等の着色剤;ハイドロキノン、カテコール、ピロガロール、フェノチアジン等の重合禁止剤;シリコーン系レベリング剤、アクリルポリマー系レベリング剤等のレベリング剤;ベントン、モンモリロナイト等の増粘剤;シリコーン系消泡剤、アクリル系消泡剤、フッ素系消泡剤、ビニル樹脂系消泡剤等の消泡剤;ベンゾトリアゾール系紫外線吸収剤等の紫外線吸収剤;尿素シラン等の接着性向上剤;トリアゾール系密着性付与剤、テトラゾール系密着性付与剤、トリアジン系密着性付与剤等の密着性付与剤;ヒンダードフェノール系酸化防止剤、ヒンダードアミン系酸化防止剤等の酸化防止剤;スチルベン誘導体等の蛍光増白剤;フッ素系界面活性剤、シリコーン系界面活性剤等の界面活性剤;リン系難燃剤(例えばリン酸エステル化合物、ホスファゼン化合物、ホスフィン酸化合物、赤リン)、窒素系難燃剤(例えば硫酸メラミン)、ハロゲン系難燃剤、無機系難燃剤(例えば三酸化アンチモン)等の非反応性ホスファゼン化合物以外の難燃剤等が挙げられる。添加剤は、1種を単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。(G)その他の添加剤の含有量は当業者であれば適宜設定できる。
本発明の樹脂組成物は、上述した不揮発性成分以外に、揮発性成分として、さらに任意の有機溶剤を含有する場合がある。(H)有機溶剤としては、公知のものを適宜用いることができ、その種類は特に限定されるものではない。(H)有機溶剤としては、例えば、アセトン、メチルエチルケトン、メチルイソブチルケトン、シクロヘキサノン等のケトン系溶剤;酢酸メチル、酢酸エチル、酢酸ブチル、酢酸イソブチル、酢酸イソアミル、プロピオン酸メチル、プロピオン酸エチル、γ-ブチロラクトン等のエステル系溶剤;テトラヒドロピラン、テトラヒドロフラン、1,4-ジオキサン、ジエチルエーテル、ジイソプロピルエーテル、ジブチルエーテル、ジフェニルエーテル等のエーテル系溶剤;メタノール、エタノール、プロパノール、ブタノール、エチレングリコール等のアルコール系溶剤;酢酸2-エトキシエチル、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、エチルジグリコールアセテート、γ-ブチロラクトン、メトキシプロピオン酸メチル等のエーテルエステル系溶剤;乳酸メチル、乳酸エチル、2-ヒドロキシイソ酪酸メチル等のエステルアルコール系溶剤;2-メトキシプロパノール、2-メトキシエタノール、2-エトキシエタノール、プロピレングリコールモノメチルエーテル、ジエチレングリコールモノブチルエーテル(ブチルカルビトール)等のエーテルアルコール系溶剤;N,N-ジメチルホルムアミド、N,N-ジメチルアセトアミド、N-メチル-2-ピロリドン等のアミド系溶剤;ジメチルスルホキシド等のスルホキシド系溶剤;アセトニトリル、プロピオニトリル等のニトリル系溶剤;ヘキサン、シクロペンタン、シクロヘキサン、メチルシクロヘキサン等の脂肪族炭化水素系溶剤;ベンゼン、トルエン、キシレン、エチルベンゼン、トリメチルベンゼン等の芳香族炭化水素系溶剤等を挙げることができる。(H)有機溶剤は、1種単独で用いてもよく、2種以上を任意の比率で組み合わせて用いてもよい。
本発明の樹脂組成物は、例えば、任意の反応容器に(A)ポリイミド樹脂(予めイミド化されているもの)、(B)シロキサン含有ポリカーボネート樹脂(予め炭酸エステル化されているもの)、必要に応じて(C)無機充填材、必要に応じて(D)エポキシ樹脂、必要に応じて(E)硬化剤、必要に応じて(F)硬化促進剤、必要に応じて(G)その他の添加剤、及び必要に応じて(H)有機溶剤を、任意の順で及び/又は一部若しくは全部同時に加えて混合することによって、製造することができる。また、各成分を加えて混合する過程で、温度を適宜設定することができ、一時的に又は終始にわたって、加熱及び/又は冷却してもよい。また、各成分を加えて混合する過程において、撹拌又は振盪を行ってもよい。また、加えて混合する際に又はその後に、樹脂組成物を、例えば、ミキサーなどの撹拌装置を用いて撹拌し、均一に分散させてもよい。
本発明の樹脂組成物は、(A)ポリイミド樹脂、及び(B)シロキサン含有ポリカーボネート樹脂を含むため、熱膨張率が低く且つ反りが抑制された硬化物を得ることができる。また、各成分の相溶性にも優れ得る。
本発明の樹脂組成物は、プリント配線板、多層フレキシブル基板等の絶縁材料、ソルダーレジスト、アンダーフィル材、ダイボンディング材、半導体封止材、穴埋め樹脂、部品埋め込み樹脂等の広範囲に使用できる。プリント配線板、多層フレキシブル基板等は、例えば、樹脂シート、プリプレグ等のシート状積層材料を用いて製造することができる。
本発明の樹脂シートは、支持体と、当該支持体上に設けられた本発明の樹脂組成物で形成された樹脂組成物層を含む。
積層シートは、複数の樹脂組成物層を積層及び硬化して製造されるシートである。積層シートは、樹脂組成物層の硬化物としての絶縁層を複数含む。通常、積層シートを製造するために積層される樹脂組成物層の数は、積層シートに含まれる絶縁層の数に一致する。積層シート1枚当たりの具体的な絶縁層の数は、通常2以上、好ましくは3以上、特に好ましくは5以上であり、好ましくは20以下、より好ましくは15以下、特に好ましくは10以下である。
積層シートは、(a)樹脂シートを準備する工程、並びに、(b)樹脂シートを用いて樹脂組成物層を複数積層及び硬化する工程を含む製造方法によって、製造できる。樹脂組成物層の積層及び硬化の順番は、所望の積層シートが得られる限り、任意である。樹脂組成物の含有成分に応じて、例えば、複数の樹脂組成物層を全て積層した後で、積層された複数の樹脂組成物層を一括して硬化させてもよい。また、例えば、ある樹脂組成物層に別の樹脂組成物層を積層する都度、その積層された樹脂組成物層の硬化を行ってもよい。
(II)第一樹脂組成物層を硬化して、第一絶縁層を形成する工程と、
(VI)第一絶縁層に、第二樹脂組成物層を積層する工程と、
(VII)第二樹脂組成物層を硬化して、第二絶縁層を形成する工程と、
を含む。また、工程(b)は、必要に応じて、
(I)シート支持基材に第一樹脂組成物層を積層する工程、
(III)第一絶縁層に、穴あけする工程、
(IV)第一絶縁層に粗化処理を施す工程、
(V)第一絶縁層上に導体層を形成する工程
等の任意の工程を含んでいてもよい。以下、各工程について説明する。
多層フレキシブル基板は、積層シートを含む。多層フレキシブル基板は、積層シートのみを含んでいてもよく、積層シートに組み合わせて任意の部材を含んでいてもよい。任意の部材としては、例えば、電子部品、カバーレイフィルムなどが挙げられる。
半導体装置は、前記の多層フレキシブル基板を備える。半導体装置は、例えば、多層フレキシブル基板と、この多層フレキシブル基板に実装された半導体チップとを備える。多くの半導体装置では、多層フレキシブル基板は、半導体装置の筐体に、その多層フレキシブル基板が含む積層シートの一方の面が向かい合うように折り曲げて収納され得る。
窒素導入管、撹拌装置を備えた500mlセパラブルフラスコに、4-アミノ安息香酸5-アミノ-1,1’-ビフェニル-2-イル9.13g(30ミリモル)、4,4’-(4,4’-イソプロピリデンジフェノキシ)ビスフタル酸二無水物15.61g(30ミリモル)、N-メチル-2-ピロリドン94.64g、ピリジン0.47g(6ミリモル)、トルエン10gを投入し、窒素雰囲気下、180℃で、途中トルエンを系外にのぞきながら4時間イミド化反応させることにより、ポリイミド樹脂1を含むポリイミド溶液(不揮発分20質量%)を得た。ポリイミド溶液において、合成したポリイミド樹脂1の析出は見られなかった。
撹拌機、分水器、温度計及び窒素ガス導入管を備えた反応容器に、芳香族テトラカルボン酸二無水物(SABICジャパン社製「BisDA-1000」、4,4’-(4,4’-イソプロピリデンジフェノキシ)ビスフタル酸二無水物)65.0g、シクロヘキサノン266.5g、及びメチルシクロヘキサン44.4gを仕込み、溶液を60℃まで加熱した。次いで、ダイマージアミン(クローダジャパン社製「PRIAMINE 1075」)43.7g、及び1,3-ビス(アミノメチル)シクロヘキサン5.4gを滴下した後、140℃で1時間かけてイミド化反応させた。これにより、ポリイミド樹脂2を含むポリイミド溶液(不揮発分30質量%)を得た。また、ポリイミド樹脂2の重量平均分子量は、25,000であった。
環流冷却器を連結した水分定量受器、窒素導入管、及び攪拌器を備えた、500mLのセパラブルフラスコを用意した。このフラスコに、4,4’-オキシジフタル酸無水物(ODPA)20.3g、γ-ブチロラクトン200g、トルエン20g、及び、5-(4-アミノフェノキシ)-3-[4-(4-アミノフェノキシ)フェニル]-1,1,3-トリメチルインダン29.6gを加えて、窒素気流下で45℃にて2時間攪拌して、反応を行った。次いで、この反応溶液を昇温し、約160℃に保持しながら、窒素気流下で縮合水をトルエンとともに共沸除去した。水分定量受器に所定量の水がたまっていること、及び、水の流出が見られなくなっていることを確認した。確認後、反応溶液を更に昇温し、200℃で1時間攪拌した。その後、冷却して、1,1,3-トリメチルインダン骨格を有するポリイミド樹脂3を含むポリイミド溶液(不揮発分20質量%)を得た。得られたポリイミド樹脂3は、下記式(X1)で表される繰り返し単位及び下記式(X2)で示す繰り返し単位を有していた。また、前記のポリイミド樹脂3の重量平均分子量は、12,000であった。
温度計、撹拌機、還流冷却器付き反応器にイオン交換水21591部、48.5%水酸化ナトリウム水溶液3674部を入れ、2,2-ビス(4-ヒドロキシフェニル)プロパン(ビスフェノールA)3880部、およびハイドロサルファイト7.6部を溶解した後、塩化メチレン14565部を加え、撹拌下22~30℃でホスゲン1900部を60分要して吹き込んだ。次に、48.5%水酸化ナトリウム水溶液1131部、p-tert-ブチルフェノール105部を塩化メチレン800部に溶解した溶液を加え、攪拌しながら下記式(4)で表されるジo-ヒドロキシフェニル末端ポリジメチルシロキサン化合物(式中の平均繰り返し数p=約37)430部を塩化メチレン1600部に溶解した溶液を、2,2-ビス(4-ヒドロキシフェニル)プロパン1モルあたり0.0008モル/分となる速度で加えて乳化状態とした後、再度激しく撹拌した。かかる攪拌下、反応液が26℃の状態でトリエチルアミン4.3部を加えて温度26~31℃において45分間撹拌を続けて反応を終了した。反応終了後、有機相を分離し、塩化メチレンで希釈して水洗した後塩酸酸性にして水洗し、水相の導電率がイオン交換水と殆ど同じになったところで温水を張ったニーダーに投入して、攪拌しながら塩化メチレンを蒸発させ、ポリカーボネート-ポリジメチルシロキサン共重合体樹脂のパウダーを得た。脱水後、熱風循環式乾燥機により120℃で12時間乾燥し、ポリカーボネート-ポリジメチルシロキサン共重合体樹脂パウダーを得た(ポリジメチルシロキサン構造含有量8.2%、ポリジメチルシロキサンドメインの平均サイズ9nm、粘度平均分子量19,400)。
ビキシレノール型エポキシ樹脂(三菱化学社製「YX4000HK」、エポキシ当量約185)5部、ナフタレン型エポキシ樹脂(新日鉄住金化学社製「ESN475V」、エポキシ当量約332)5部、ビスフェノールAF型エポキシ樹脂(三菱化学社製「YL7760」、エポキシ当量約238)10部、シクロヘキサン型エポキシ樹脂(三菱化学社製「ZX1658GS」、エポキシ当量約135)2部、合成例1で得たポリイミド溶液(不揮発成分20質量%)100部、及びシクロヘキサノン10部の混合溶剤に撹拌しながら加熱溶解させた。室温にまで冷却した後、そこへ、合成例4で得たポリカーボネート-ポリジメチルシロキサン共重合体樹脂(不揮発成分20質量%、トルエン溶液)50部、トリアジン骨格含有クレゾールノボラック系硬化剤(DIC社製「LA3018-50P」、水酸基当量約151、固形分50%の2-メトキシプロパノール溶液)4部、活性エステル系硬化剤(DIC社製「EXB-8000L-65M」、活性基当量約220、不揮発成分65質量%のトルエン:MEKの1:1溶液)6部、球形シリカ(アドマテックス社製「SC2500SQ」、平均粒径0.5μm、比表面積11.2m2/g、シリカ100部に対してN-フェニル-3-アミノプロピルトリメトキシシラン(信越化学工業社製、KBM573)1部で表面処理したもの)50部、アミン系硬化促進剤(4-ジメチルアミノピリジン(DMAP))0.2部を混合し、高速回転ミキサーで均一に分散した後に、カートリッジフィルター(ROKITECHNO社製「SHP020」)で濾過して、樹脂組成物1を調製した。
合成例1で得たポリイミド溶液(不揮発成分20質量%)100部を使用する代わりに、合成例2で得たポリイミド溶液(不揮発成分30質量%)66.7部を使用したこと以外、実施例1と同じ操作を行って、樹脂組成物2を調製した。
合成例1で得たポリイミド溶液(不揮発成分20質量%)100部を使用する代わりに、合成例3で得たポリイミド溶液(不揮発成分20質量%)100部を使用したこと以外、実施例1と同じ操作を行って、樹脂組成物3を調製した。
合成例4で得たポリカーボネート-ポリジメチルシロキサン共重合体樹脂(不揮発成分20質量%、トルエン溶液)50部を使用する代わりに、ポリカーボネート樹脂(三菱ガス化学社製「FPC2136」、不揮発分20質量%)50部を使用したこと以外は、実施例1と同じ操作を行って、樹脂組成物4を調製した。
合成例4で得たポリカーボネート-ポリジメチルシロキサン共重合体樹脂(不揮発成分20質量%、トルエン溶液)50部を使用しなかったこと、及びエポキシ変性シリコーンオイル(信越化学社製「KF-105」)10部を使用したこと以外は、実施例1と同じ操作を行って、樹脂組成物5を調製した。
合成例4で得たポリカーボネート-ポリジメチルシロキサン共重合体樹脂(不揮発成分20質量%、トルエン溶液)50部を使用する代わりに、ポリカーボネート樹脂(三菱ガス化学社製「FPC2136」、不揮発分20質量%)50部を使用したこと、及びエポキシ変性シリコーンオイル(信越化学社製「KF-105」)10部を使用したこと以外は、実施例1と同じ操作を行って、樹脂組成物6を調製した。
合成例1で得たポリイミド溶液(不揮発成分20質量%)100部を使用する代わりに、フェノキシ樹脂(三菱ケミカル社製「YX7553BH30」、不揮発成分30質量%、MEKとシクロヘキサノンの1:1溶液)66.67部を使用したこと以外は、実施例1と同じ操作を行って、樹脂組成物7を調製した。
無機充填材100mg、及びメチルエチルケトン10gをバイアル瓶に秤取り、超音波にて10分間分散した。レーザー回折式粒径分布測定装置(堀場製作所社製「LA-960」)を使用して、使用光源波長を青色および赤色とし、フローセル方式で無機充填材の粒径分布を体積基準で測定した。得られた粒径分布から、メディアン径として、無機充填材の平均粒径を算出した。
BET全自動比表面積測定装置(マウンテック社製Macsorb HM-1210)を使用して、試料表面に窒素ガスを吸着させ、BET多点法を用いて比表面積を算出することで無機充填材の比表面積を測定した。
調整した樹脂組成物1~6を5℃の冷蔵庫内に3日保存し、その後樹脂組成物をガラスプレート上に塗布した後、脂組組成物中の分離の有無を光学顕微鏡(ハイロックス社製「KH8700」)で観察した。光学顕微鏡にて分離物の発生が確認できなかった場合を「○」と評価し、分離物の発生が確認できた場合を「×」と評価した。
各実施例及び比較例の樹脂組成物をアルキド系離型剤で処理されたPETフィルム(厚さ38μm)の離型処理面上に、乾燥後の樹脂組成物層の厚さが40μmになるよう、ダイコータにて均一に塗布し、80~120℃(平均100℃)で6分間乾燥させて、樹脂シート1を得た。
各実施例及び比較例の樹脂組成物をアルキド系離型剤で処理されたPETフィルム(厚さ38μm)の離型処理面上に、乾燥後の樹脂組成物層の厚さが30μmになるよう、ダイコータにて均一に塗布し、80~120℃(平均100℃)で6分間乾燥させて、樹脂シート2を得た。
Claims (16)
- (A)ポリイミド樹脂、(B)シロキサン含有ポリカーボネート樹脂、(C)シリカ、及び(D)エポキシ樹脂を含み、
(A)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、15質量%以上であり
(B)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、1質量%以上30質量%以下であり、
(C)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、40質量%以上であり、
(D)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、10質量%以上である、樹脂組成物。 - (A)成分の重量平均分子量が、1,000以上100,000以下である、請求項1に記載の樹脂組成物。
- (B)成分が、ポリカーボネート構造を有するポリカーボネートブロックと、ポリシロキサン構造を有するポリシロキサンブロックと、を含むポリカーボネート-ポリシロキサン共重合体である、請求項1に記載の樹脂組成物。
- ポリシロキサン構造が、ポリジアルキルシロキサン構造である、請求項3に記載の樹脂組成物。
- ポリカーボネート構造が、芳香族ポリカーボネート構造である、請求項3に記載の樹脂組成物。
- (B)成分中のポリシロキサン構造の含有量が、(B)成分を100質量%とした場合、1質量%以上30質量%以下である、請求項3に記載の樹脂組成物。
- (B)成分の粘度平均分子量が、13,000以上25,000以下である、請求項1に記載の樹脂組成物。
- (A)成分と(B)成分の質量比((A)成分/(B)成分)が、1以上5以下である、請求項1に記載の樹脂組成物。
- (C)成分の含有量が、樹脂組成物中の不揮発成分を100質量%とした場合、60質量%以下である、請求項1に記載の樹脂組成物。
- さらに(E)硬化剤を含む、請求項1に記載の樹脂組成物。
- (E)成分が、活性エステル系硬化剤を含む、請求項10に記載の樹脂組成物。
- 多層フレキシブル基板の絶縁層形成用である、請求項1に記載の樹脂組成物。
- 請求項1~11の何れか1項に記載の樹脂組成物の硬化物。
- 支持体と、当該支持体上に設けられた請求項1~11の何れか1項に記載の樹脂組成物で形成された樹脂組成物層とを含む、樹脂シート。
- 請求項1~11の何れか1項に記載の樹脂組成物を硬化して形成される絶縁層を含む多層フレキシブル基板。
- 請求項15に記載の多層フレキシブル基板を備える、半導体装置。
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