JP4872125B2 - 多層プリント配線板用硬化性樹脂組成物、熱硬化性接着フィルム及び多層プリント基板 - Google Patents
多層プリント配線板用硬化性樹脂組成物、熱硬化性接着フィルム及び多層プリント基板 Download PDFInfo
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- JP4872125B2 JP4872125B2 JP2006177965A JP2006177965A JP4872125B2 JP 4872125 B2 JP4872125 B2 JP 4872125B2 JP 2006177965 A JP2006177965 A JP 2006177965A JP 2006177965 A JP2006177965 A JP 2006177965A JP 4872125 B2 JP4872125 B2 JP 4872125B2
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Description
(1)フェノール系化合物の構造残基とフェノール性水酸基とイソシアネート基との反応にて生成されるウレタン結合とを有するポリイミド樹脂とエポキシ樹脂を含有する樹脂組成物を用いて得られる硬化物は、耐熱性、電気特性、機械物性、寸法安定性に優れる。
本発明は上記の知見を基に完成したものである。
(1)塗布乾燥後に生じる凹凸をフラットにする、
(2)研磨後に行なう表面の粗化工程での薬品のアタックを容易にする(表面濡れ性向上)、
(3)膜厚を希望の厚みに薄くする、
ことであるが、硬化後に充分な平坦性や膜厚がある場合等、必要ないと判断できる際には研磨しなくてもよい。このとき、使用できる研磨の種類としては、ベルトサンダー、パフ、ナイロンブラシ等がある。
(1)基板全面に無電解の金属めっきを施し、さらに電解めっきにて金属めっき層を形成した後、形成したいパターン通りに市販のネガ型パターンレジスト又はポジ型パターンレジストのパターンを形成する。その後、金属をエッチングすることにより、最外層の導体パターンを得るパネルめっき法、
(2)塗膜表面上に逆パターンの永久めっきレジストを形成し、そのレジストが形成されていない部分に無電解めっきにて導体パターンを形成するアディティブ法、
(3)上記(1)の方法と同様、基板全体に無電解金属めっきを施した後、逆パターンのネガ型又はポジ型めっきレジストのバターンを形成する。その後、電解めっきにてレジストのパターンが存在しない部分に選択的にめっき層を形成させる。次いで、パターンレジストを剥離し、パターンレジストに隠されていた無電解めっき層をエッチングすることにより導体パターンを得るセミアディティブ法、
などがある。
熱硬化性樹脂組成物を用いた場合、基板上に形成した乾燥塗膜上に、片面もしくは両面に粗面を有する銅箔又は樹脂付き銅箔を前述した第一の形態で説明した真空フィルムラミネ一夕ーで加熱ラミネートして一体成形する。また、必着に応じて、真空フィルムラミネ一夕ーで銅箔又は樹脂付き銅箔を加熱ラミネートした後、さらに熱板プレス機にて塗膜を加熱加圧してレベリング(平坦化)することが好ましい。
基板上に形成した乾燥塗膜上に、片面もしくは両面に粗面を有する銅箔又は樹脂付き銅箔を重ね合せ、熱板プレス機で加熱加圧して一体成形を行なう。プレスの条件としては、機械の性能により多少異なるが、140〜200℃で1〜4時間、圧力15〜50kg/cm2の範囲で行なう。この際、プリプレグや接着シートを介して銅箔を乾燥塗膜に接着することもできる。
攪拌装置、温度計およびコンデンサーを付けたフラスコに、DMAC(ジメチルアセトアミド)140gと、TMEG(エチレングリコールビスアンヒドロトリメリテート)98.4g(0.24モル)と、BPS(ビスフェノールS)40g(0.16モル)と、MDI(ジフェニルメタンジイソシアネート)40g(0.16モル)とHDI(ヘキサメチレンジイソシアネート)26.9g(0.16モル)を仕込み、攪拌を行いながら発熱に注意して80℃に昇温し、この温度で1時間かけて溶解、反応させ、更に2時間かけて120℃まで昇温した後、この温度で1時間反応させた。反応は炭酸ガスの発泡とともに進行し、系内は茶色の液体となった。 DMACにて樹脂固形分濃度を55%に調整し、25℃での粘度が100Pa・sのポリイミド樹脂(X−1)の溶液を得た。
攪拌装置、温度計およびコンデンサーを付けたフラスコに、DMAC 156.8gと、TMEG 65.6g(0.16モル)と、BP(ビフェノール)29.8g(0.16モル)と、MDI 40g(0.16モル)と、1,6−ヘキサンジイソシアネートから誘導されるイソシアヌレート環を有するポリイソシアネート(以下、HDI−Nと略記する。イソシアネート基含有率23.5%、イソシアヌレート環含有トリイソシアネート含有率63.3%)21.4g(イソシアネート基として0.12モル)を仕込み、攪拌を行いながら発熱に注意して100℃に昇温し、この温度で7時間反応させた。反応は発泡とともに進行し、系内はクリアな茶色の液体となった。25℃での粘度が15Pa・sのポリイミド樹脂(X−2)の溶液を得た。
攪拌装置、温度計およびコンデンサーを付けたフラスコに、γ−ブチロラクトン 184gと、TMEG 82.0g(0.2モル)と、BPF(ビフェノールF)40.4g(0.2モル)と、TDI(トリレンジイソシアネート) 34.8g(0.2モル)と、1,6−ヘキサンジイソシアネートから誘導されるイソシアヌレート環を有するポリイソシアネート(以下、HDI−Nと略記する。イソシアネート基含有率23.5%、イソシアヌレート環含有トリイソシアネート含有率63.3%)26.8g(イソシアネート基として0.15モル)を仕込み、攪拌を行いながら発熱に注意して120℃に昇温し、この温度で7時間反応させた。反応は発泡とともに進行し、系内はクリアな茶色の液体となった。 25℃での粘度が7Pa・sのポリイミド樹脂(X−3)の溶液を得た。
攪拌装置、温度計およびコンデンサーを付けた20リットルのフラスコに、ジエチレングリコールモノエチルエーテルアセテート4951gと、IPDI−N2760g(イソホロンジイソシアネートのイソシアヌレート化合物、NCO含有率18.26%、イソシアネート基として12モル)と、ポリテールHA〔三菱化学(株)製の両末端に水酸基を有する水素添加液状ポリブタジエン、数平均分子量2,100、水酸基価51.2mgKOH/g〕2191g(水酸基として2モル)を仕込み、攪拌を行いながら発熱に注意して80℃に昇温した後、3時間反応を行った。次いで、さらにジエチレングリコールモノエチルエーテルアセテート1536gとトリメリット酸無水物1536g(8モル)を仕込み、160℃まで昇温した後、4時間反応させた。反応は発泡とともに進行した。系内は薄茶色のクリアな液体となり、ポリイミド樹脂(X′−1)の溶液を得た。
第1表及び第2表に示す配合にて熱硬化性樹脂組成物1〜4及び比較対照用熱硬化性樹脂組成物1及び2を調製した。表中の数値はいずれも固形換算分での配合量(重量部)を表す。得られた樹脂組成物のチキソトロビックインデックス(TI倍)は、すべて1.2〜2.0の範囲内であった。
前記実施例1〜4及び比較例1〜3で得られた熱硬化性樹脂組成物をそれぞれ、ロールコーターを用いて、フィルムの膜厚が50μmになるようにPETフィルム(東レ株式会社製、ルミラー38R75:38μm)に塗布し、40〜120℃で乾燥して接着フィルムを得た。このとき150℃におけるゲル化タイムはすべてのサンプルにおいて20秒から120秒の範囲内であった。
前記実施例1〜4及び比較例1〜3で得られた熱硬化性樹脂組成物をそれぞれ、銅箔(35μm)にスクリーン印刷し、110℃で30分乾燥し、次いで150℃×30分さらに170℃×30分の条件で最終硬化させた。この試料の銅箔をエッチングし、それぞれの硬化皮膜として物性を測定した。結果を第3表に示す。
TMA(熱機械分析)により測定した。
TMAにより測定した。
JIS K6911に従って測定した。
硬化皮膜を23℃±2℃に管理された蒸留水に浸漬し、24時間後の重量変化より求めた。
前記実施例1〜4及び比較例1〜3で得られた熱硬化性樹脂組成物をそれぞれ、1000μmの溝ピッチを有するウレタンゴム製ロールを備えた垂直吊り上げ式ロールコーター(ファーネス社製)を用いて、銅箔18μm厚のガラスエポキシ両面銅張積層板から内層回路を形成し、さらにエッチボンド(メック社製)処理した基板の両面に同時に塗布し、次いで110℃で乾燥し、絶縁層となる乾燥塗膜を形成した。
JIS C6481に従って測定した。
288℃±3℃のはんだ層に、完成したプリント配線板(10cm×lOcm)を10秒間浸漬する。この操作を5回線り返した後、銅箔と樹脂の剥がれを確認した。なお、表4中の符号の意味は以下のとおりである。
OK:剥がれ無し。
NG:剥がれ有り。
ラインアンドスペース75μm/75μmの回路の剥がれを目視で検査した。なお、表4中の符号の意味は以下のとおりである。
OK:剥がれ無し。
NG:剥がれ有り。
0.4mmの厚さのFR−4基材に硬化塗膜で80μmになるように両面に絶縁層を形成し、UL−94に従い試験を行なった。なお、表4中の符号の意味は以下のとおりである。
NG:サンプル片の炎がクランプまで達し、ULー94のV0不適合である。
前記試験例1の基板作成において、ポストキュアー後に#320相当と#600相当のパフ研磨を2回繰り返した以外は同様に作成した基板の第3表及び第4表に示した、物性、特性を評価した。結果は第3表、第4表に示した結果とほぼ同様で、さらに内層回路の凹凸に伴う基板表面の凹凸が減少していることが確認された。
前記試験例2の基板作成において、パネルめっき法をセミアディティブ法に変更して作成した以外は同様に作成した基板の第4表に示した特性を評価した。結果は第4表に示した結果とほぼ同様でさらにライン/スペース=25μm/25μmの回路が形成でき、剥がれが生じていなかった。
次に、前述したプリント配線板の製造方法の第二の形態に従い、前記実施例1〜4及び比較例1〜3の熱硬化性樹脂組成物の乾燥塗膜を形成した基板の両面に18μm厚の銅箔(ジャパンエナジー社製)を重ね、真空ラミネ一夕ー(MEIKl社製、MVLP−500)を用い、5kgf/cm2、150℃、1分、1Torrの条件にて加熱ラミネートし、次いで熱板プレス機で10kgf/cm2、150℃、1分の条件にてレベリングした後、熱風循環式乾燥機で170℃×30分の条件にて硬化させ、積層板を作製した。
前記実施例5〜8及び比較例4〜6で作製した接着フィルムを、35μmの銅箔に真空ラミネ一夕ー(MEIKl社製、MVLP−500)を用いて5kgf/cm2、140℃、1分、1Torrの条件にて加熱ラミネートし、次いで熱板プレス機で10kgf/cm2、150℃、1分の条件にてレベリングした後、PETフィルムを剥離して熱風循環式乾燥機で150℃×60分さらに170℃×30分の条件で硬化させた。そして、得られたサンプルの銅箔を市販のエッチング液でエッチングし、前記試験例1と同様にして物性の評価を行なった。結果を表6に示す。
次に、前述したプリント配線板の製造方法の第一の形態に従い、前記実施例5〜8及び比較例4〜6で作製した接着フィルムを、銅箔18μm厚のガラスエポキシ両面銅張積層板から内層回路を形成し、さらにエッチボンド(メック社製)処理した基板の両面に、真空ラミネ一夕ー(MEIKI社製、MVLP−500)を用い、5kgf/cm2、140℃、1分、1Torrの条件にて加熱ラミネートし、次いで熱板プレス機で10kgf/cm2、150℃、1分の条件にてレベリングした後、熱風循頻式乾燥機で150℃×60分の条件にて硬化させ、積層板を作製した。
前記実施例5〜8の基板作製においてパネルめっき法をセミアディティブ法に変更して作製した基板の特性はほぼ上記と同等で、さらにライン/スペース=25μm/25μmの回路が形成でき、剥がれが生じていなかった。
次に、前述したプリント配擦板の製造方法の第一の形態に従い、前記実施例5〜8及び比較例4〜6で作製した接着フィルムをラミネートした積層板の支持フィルムを剥離し、18μm厚の銅箔(ジャパンエナジー社製JTC−AM)を重ね、真空ラミネ一夕ー(MEIKI社製、MVLP−500)を用い、5kgf/cm2、150℃、1分、1Torrの条件にて加熱ラミネートし、次いで熱板プレス機で10kgf/cm2、150℃、1分の条件にてレベリングした後、熱風循衆式乾燥機で170℃×30分の条件にて硬化させ、積層板を作製した。
Claims (16)
- 前記エポキシ樹脂(B)が芳香族系エポキシ樹脂である請求項1〜4のいずれか1項記載の熱硬化性樹脂組成物。
- 硬化触媒を含有する請求項1〜4のいずれか1項記載の熱硬化性樹脂組成物。
- 更に、ウレタン化触媒を含有する請求項1〜4のいずれか1項記載の熱硬化性樹脂組成物。
- 前記エポキシ樹脂(B)が芳香族系エポキシ樹脂である請求項8〜11のいずれか1項記載の熱硬化性接着フイルム。
- 硬化触媒を含有する請求項8〜12のいずれか1項記載の熱硬化性接着フイルム。
- 更に、ウレタン化触媒を含有する請求項8〜12のいずれか1項記載の熱硬化性接着フイルム。
- 請求項1〜7のいずれか1項記載の熱硬化性樹脂組成物を用いて層間絶縁樹脂層が形成されていることを特徴とする多層プリント基板。
- 請求項8〜14のいずれか1項記載の熱硬化性接着フイルムを用いて層間絶縁樹脂層が形成されていることを特徴とする多層プリント基板。
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