JP2017019970A - 樹脂組成物 - Google Patents
樹脂組成物 Download PDFInfo
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- JP2017019970A JP2017019970A JP2015140710A JP2015140710A JP2017019970A JP 2017019970 A JP2017019970 A JP 2017019970A JP 2015140710 A JP2015140710 A JP 2015140710A JP 2015140710 A JP2015140710 A JP 2015140710A JP 2017019970 A JP2017019970 A JP 2017019970A
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- epoxy resin
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- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 1
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Landscapes
- Reinforced Plastic Materials (AREA)
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Abstract
Description
本発明が解決しようとする課題は、粗度が低くても導体層に対し高いピール強度を示し、かつ誘電正接の低い絶縁層を達成し得る樹脂組成物を提供することである。
[1] (A)エポキシ樹脂と、(B)トリアジン構造を含有する活性エステル化合物と、を含む樹脂組成物。
[2] (A)エポキシ樹脂の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、0.1質量%〜30質量%である[1]に記載の樹脂組成物。
[3] (B)トリアジン構造を含有する活性エステル化合物の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、0.1質量%〜30質量%である[1]又は[2]に記載の樹脂組成物。
[4] (B)トリアジン構造を有する活性エステル化合物が下記式(1)である、[1]〜[3]のいずれかに記載の樹脂組成物。
R1は、アミノ基、アルキル基、アリール基、アルコキシ基、水素原子、又はハロゲン原子を表し、R2は、1価の芳香族基、1価の脂肪族基、又は1価の脂環式基を表し、
Ar1及びAr2は、それぞれ独立に、置換基を有していてもよい3価の芳香族基を表し、j及びkは、それぞれ正の数を表し、lは0以上の数を表す)
[5] (C)無機充填材を含む[1]〜[4]のいずれかに記載の樹脂組成物。
[6] (C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、50質量%以上である[5]に記載の樹脂組成物。
[7] 熱硬化により形成される絶縁層の誘電正接が0.008以下である〔1〕〜〔6〕のいずれかに記載の樹脂組成物。
[8] 支持体と、該支持体上に設けられた[1]〜[7]のいずれかに記載の樹脂組成物を含む樹脂組成物層と、を有する接着フィルム。
[9] [1]〜[7]のいずれかに記載の樹脂組成物がシート状繊維基材中に含浸されたプリプレグ。
[10] [1]〜[7]のいずれかに記載の樹脂組成物の硬化物により形成された絶縁層を含むプリント配線板。
[11] [10]に記載のプリント配線板を含む、半導体装置。
本発明の樹脂組成物は、(A)エポキシ樹脂と、(B)トリアジン構造を含有する活性エステル化合物と、を含む。以下、本発明の樹脂組成物に含まれる各成分について詳細に説明する。
本発明の樹脂組成物は、(A)エポキシ樹脂(以下、「(A)成分」ともいう)を含有する。
したがって樹脂組成物中の(A)成分の含有量は、好ましくは0.1〜30質量%、より好ましくは5〜25質量%、さらに好ましくは10〜22質量%である。
本発明の樹脂組成物は、(B)トリアジン構造を含有する活性エステル化合物(以下、「トリアジン構造含有活性エステル化合物」、「(B)成分」ともいう)を含有する。
R1は、アミノ基、アルキル基、アリール基、アルコキシ基、水素原子、又はハロゲン原子を表し、R2は、1価の芳香族基、1価の脂肪族基、又は1価の脂環式基を表し、
Ar1及びAr2は、それぞれ独立に、置換基を有していてもよい3価の芳香族基を表し、j及びkは、それぞれ正の数を表し、lは0以上の数を表す)
したがって樹脂組成物中の(B)成分の含有量は、好ましくは0.1〜30質量%、より好ましくは1〜25質量%、さらに好ましくは5〜20質量%である。
本発明の樹脂組成物は(B)成分とともに(B)成分以外の硬化剤を含んでいてもよい。
(B)成分以外の硬化剤としては、エポキシ樹脂を硬化する機能を有する限り特に限定されないが、例えば、フェノール系硬化剤、ナフトール系硬化剤、活性エステル系硬化剤、ベンゾオキサジン系硬化剤、シアネートエステル系硬化剤及びカルボジイミド系硬化剤が挙げられる。硬化剤は1種単独で用いてもよく、又は2種以上を併用してもよい。
本発明の樹脂組成物は、(C)無機充填材(以下、「(C)成分」ともいう)を含有していてもよい。
無機充填材の材料は特に限定されないが、例えば、シリカ、アルミナ、ガラス、コーディエライト、シリコン酸化物、硫酸バリウム、炭酸バリウム、タルク、クレー、雲母粉、酸化亜鉛、ハイドロタルサイト、ベーマイト、水酸化アルミニウム、水酸化マグネシウム、炭酸カルシウム、炭酸マグネシウム、酸化マグネシウム、窒化ホウ素、窒化アルミニウム、窒化マンガン、ホウ酸アルミニウム、炭酸ストロンチウム、チタン酸ストロンチウム、チタン酸カルシウム、チタン酸マグネシウム、チタン酸ビスマス、酸化チタン、酸化ジルコニウム、チタン酸バリウム、チタン酸ジルコン酸バリウム、ジルコン酸バリウム、ジルコン酸カルシウム、リン酸ジルコニウム、及びリン酸タングステン酸ジルコニウム等が挙げられる。これらの中でもシリカが特に好適である。またシリカとしては球状シリカが好ましい。無機充填材は1種単独で用いてもよく、2種以上を組み合わせて用いてもよい。無機充填材の市販品としては、例えば(株)アドマテックス製「SO−C2」、「SO−C1」等が挙げられる。
熱可塑性樹脂としては、例えば、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、ポリブタジエン樹脂、ポリイミド樹脂、ポリアミドイミド樹脂、ポリエーテルイミド樹脂、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、ポリカーボネート樹脂、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が挙げられ、これらのうち、フェノキシ樹脂が好ましい。熱可塑性樹脂は、1種単独で用いてもよく、又は2種以上を組み合わせて用いてもよい。
硬化促進剤としては、例えば、リン系硬化促進剤、アミン系硬化促進剤、イミダゾール系硬化促進剤、グアニジン系硬化促進剤等が挙げられ、リン系硬化促進剤、アミン系硬化促進剤、イミダゾール系硬化促進剤が好ましく、アミン系硬化促進剤、イミダゾール系硬化促進剤がより好ましい。硬化促進剤は、1種単独で用いてもよく、2種以上を組み合わせて用いてもよい。
本発明の樹脂組成物は、難燃剤を含んでもよい。難燃剤としては、例えば、有機リン系難燃剤、有機系窒素含有リン化合物、窒素化合物、シリコーン系難燃剤、金属水酸化物等が挙げられる。難燃剤は1種単独で用いてもよく、又は2種以上を併用してもよい。
樹脂組成物は、さらに有機充填材を含んでもよい。有機充填材としては、プリント配線板の絶縁層を形成するに際し使用し得る任意の有機充填材を使用してよく、例えば、ゴム粒子、ポリアミド微粒子、シリコーン粒子等が挙げられ、ゴム粒子が好ましい。
本発明の接着フィルムは、支持体と、該支持体上に設けられた、本発明の樹脂組成物を含む樹脂組成物層と、を有する。
本発明のプリプレグは、本発明の樹脂組成物が、シート状繊維基材中に含浸されていることを特徴とする。
本発明のプリント配線板は、本発明の樹脂組成物の硬化物により形成された絶縁層を含むことを特徴とする。
(I)内層基板上に、接着フィルムを、該接着フィルムの樹脂組成物層が内層基板と接合するように積層する工程
(II)樹脂組成物層を熱硬化して絶縁層を形成する工程
本発明の半導体装置は、プリント配線板を含むことを特徴とする。本発明の半導体装置は、本発明のプリント配線板を用いて製造することができる。
液状ビスフェノールA型エポキシ樹脂(、三菱化学(株)製「828US」、エポキシ当量190)15部と、ビフェニルアラルキル型エポキシ樹脂(エポキシ当量291、日本化薬(株)製「NC3000H」)15部とをメチルエチルケトン(以下「MEK」と略称する。)5部、シクロヘキサノン5部に撹拌しながら加熱溶解させた。そこへ、トリアジン構造含有活性エステル化合物(DIC(株)製「EXB9510」、活性エステル当量214)を不揮発分60%となるようにMEKに溶解させた溶液を25部、硬化促進剤(広栄化学工業(株)製、「4−ジメチルアミノピリジン」)0.1部、球形シリカ(平均粒径0.5μm、フェニルアミノシラン処理付「SO−C2」、(株)アドマテックス製、単位重量あたりのカーボン量0.18%)100部、フェノキシ樹脂(YX6954BH30、固形分30質量%のMEK及びシクロヘキサノン溶液、重量平均分子量35000)15部を混合し、高速回転ミキサーで均一に分散して、樹脂ワニスを作製した。次に、かかる樹脂ワニスをポリエチレンテレフタレート(厚さ38μm、以下「PET」と略称する。)上に、乾燥後の樹脂厚みが40μmとなるようにダイコーターにて塗布し、80〜120℃(平均100℃)で6分間乾燥させて、シート状の接着フィルムを得た。
実施例1のトリアジン構造含有活性エステル化合物(DIC(株)製「EXB9510」、活性エステル当量214、不揮発分60%のMEK溶液)を、トリアジン構造含有活性エステル化合物(DIC(株)製「EXB9511」、活性エステル当量240)を不揮発分60%となるようにMEKに溶解させた溶液)に変更した以外は、実施例1と同様にして樹脂ワニスを作成し、接着フィルムを得た。
実施例1の液状ビスフェノールA型エポキシ樹脂(三菱化学(株)製「828US」、エポキシ当量190)15部をナフタレン型エポキシ樹脂(DIC(株)製「EXA4032SS」、エポキシ当量143)10部に変更するとともに、ビフェニルアラルキル型エポキシ樹脂(日本化薬(株)製「NC3000H」、エポキシ当量291)15部をナフトールアラルキル型エポキシ樹脂(新日鉄住金化学(株)製「ESN475V」、エポキシ当量331)15部に変更したこと以外は、実施例1と同様にして樹脂ワニスを作製し、接着フィルムを得た。
実施例2の液状ビスフェノールA型エポキシ樹脂(三菱化学(株)製「828US」、エポキシ当量190)15部をナフタレン型エポキシ樹脂(DIC(株)製「EXA4032SS」、エポキシ当量143)10部に変更するとともに、ビフェニルアラルキル型エポキシ樹脂(日本化薬(株)製「NC3000H」、エポキシ当量291)15部をナフトールアラルキル型エポキシ樹脂(新日鉄住金化学(株)製「ESN475V」、エポキシ当量331)15部に変更したこと以外は、実施例2と同様にして樹脂ワニスを作製し、接着フィルムを得た。
実施例3のトリアジン構造含有活性エステル化合物(DIC(株)製「EXB−9510」、活性エステル当量214)を、トリアジン構造を含有しない活性エステル化合物(DIC(株)製「HPC−8000−65T」、活性エステル当量223、不揮発分65%のトルエン溶液)20部に変更したこと以外は、実施例3と同様にして樹脂ワニスを作製し、接着フィルムを得た。
実施例3のトリアジン構造含有活性エステル化合物(DIC(株)製「EXB−9510」、活性エステル当量214)を、トリアジン構造含有フェノールノボラック化合物(DIC(株)製「LA7052」、フェノール性水酸基当量120、不揮発分60%のMEK溶液)15部に変更するとともに、フェニルアミノシラン処理付「SO−C2」、(株)アドマテックス製、単位重量あたりのカーボン量0.18%)の添加量を65部としたこと以外は、実施例3と同様にして樹脂ワニスを作製し、接着フィルムを得た。
実施例3のトリアジン構造含有活性エステル化合物(DIC(株)製「EXB−9510」、活性エステル当量214)を、トリアジン構造含有フェノールノボラック化合物(DIC(株)製「LA7052」、フェノール性水酸基当量120、不揮発分60%のMEK溶液)10部及びトリアジン構造を含有しない活性エステル化合物(DIC(株)製「HPC−8000−65T」、活性エステル当量223、不揮発分65%のトルエン溶液)5部に変更するとともに、フェニルアミノシラン処理付「SO−C2」、(株)アドマテックス製、単位重量あたりのカーボン量0.18%)の添加部数を65部としたこと以外は、実施例3と同様にして樹脂ワニスを作製し、接着フィルムを得た。
以下、各評価試験における測定方法・評価方法について説明する。
(1)積層板の下地処理
内層回路の形成されたガラス布基材エポキシ樹脂両面銅張積層板(銅箔の厚さ18μm、残銅率60%、基板厚み0.3mm、松下電工(株)製R5715ES)両面をメック(株)製CZ8100に浸漬して銅表面の粗化処理をおこなった。
各実施例及び各比較例で作成した接着フィルムを、バッチ式真空加圧ラミネーターMVLP-500((株)名機製作所製、商品名)を用いて、積層板の両面にラミネートした。ラミネートは、30秒間減圧して気圧を13hPa以下とし、その後30秒間、100℃、圧力0.74MPaで圧着させることにより行った。
ラミネートされた接着フィルムからPETフィルムを剥離し、170℃、30分の硬化条件で樹脂組成物を硬化した。
積層板を、膨潤液である、アトテックジャパン(株)のジエチレングリコールモノブチルエーテル含有のスエリングディップ・セキュリガンドPに60℃で10分間浸漬し、次に粗化液として、アトテックジャパン(株)のコンセントレート・コンパクトP(KMnO4:60g/L、NaOH:40g/Lの水溶液)に80℃で20分間浸漬、最後に中和液として、アトテックジャパン(株)のリダクションショリューシン・セキュリガントPに40℃で5分間浸漬した。この粗化処理後の積層板をサンプルAとした。
絶縁層表面に回路を形成するために、積層板を、PdCl2を含む無電解メッキ用溶液に浸漬し、次に無電解銅メッキ液に浸漬した。150℃にて30分間加熱してアニール処理を行った後に、エッチングレジストを形成し、エッチングによるパターン形成の後に、硫酸銅電解メッキを行い、30μmの厚さで導体層を形成した。次に、アニール処理を180℃にて60分間行った。この積層板をサンプルBとした。
サンプルAについて、非接触型表面粗さ計(ビーコインスツルメンツ社製WYKO NT3300)を用いて、VSIコンタクトモード、50倍レンズにより測定範囲を121μm×92μmとして得られる数値により算術平均粗さ(粗度)を求めた。そして、それぞれ10点の平均値を求めることにより測定値とし、表1に示した。
サンプルBの導体層に、幅10mm、長さ100mmの部分の切込みをいれ、この一端を剥がしてつかみ具((株)ティー・エス・イー、オートコム型試験機 AC−50C−SL)で掴み、室温中にて、50mm/分の速度で垂直方向に35mmを引き剥がした時の荷重(kgf/cm)を測定し、表1に示した。
各実施例および各比較例で得られた接着フィルムを190℃で90分熱硬化させて、PETフィルムを剥離してシート状の硬化物を得た。その硬化物を、幅2mm、長さ80mmの試験片に切断し、関東応用電子開発(株)製空洞共振器摂動法誘電率測定装置CP521およびアジレントテクノロジー(株)製ネットワークアナライザーE8362Bを使用して、空洞共振法で測定周波数5.8GHzにて誘電正接(tanδ)の測定を行った。2本の試験片について測定を行い、平均値を算出し、表1に示した。
Claims (11)
- (A)エポキシ樹脂と、(B)トリアジン構造を含有する活性エステル化合物と、を含む樹脂組成物。
- (A)エポキシ樹脂の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、0.1質量%〜30質量%である請求項1に記載の樹脂組成物。
- (B)トリアジン構造を含有する活性エステル化合物の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、0.1質量%〜30質量%である請求項1又は2に記載の樹脂組成物。
- (C)無機充填材を含む請求項1〜4のいずれか1項に記載の樹脂組成物。
- (C)無機充填材の含有量が、樹脂組成物中の不揮発成分を100質量%としたとき、50質量%以上である請求項5に記載の樹脂組成物。
- 熱硬化により形成される絶縁層の誘電正接が0.008以下である請求項1〜6のいずれか1項に記載の樹脂組成物。
- 支持体と、該支持体上に設けられた請求項1〜7のいずれか1項に記載の樹脂組成物を含む樹脂組成物層と、を有する接着フィルム。
- 請求項1〜7のいずれか1項に記載の樹脂組成物がシート状繊維基材中に含浸されたプリプレグ。
- 請求項1〜7のいずれか1項に記載の樹脂組成物の硬化物により形成された絶縁層を含むプリント配線板。
- 請求項10に記載のプリント配線板を含む、半導体装置。
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |