JPWO2016063506A1 - 樹脂組成物、プリプレグ、樹脂付き金属箔、金属張積層板及びプリント配線板 - Google Patents
樹脂組成物、プリプレグ、樹脂付き金属箔、金属張積層板及びプリント配線板 Download PDFInfo
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Abstract
Description
={1−(A2/B2)/(A1/B1)}×100
酸無水物の開環率が80%未満である場合、未反応の酸無水物が多く残存し、プリプレグの製造中に酸無水物が揮発して消失しやすい。揮発により硬化剤が不足し、樹脂組成物の硬化物の架橋密度が低下することが考えられる。架橋密度が低下することにより、硬化物のガラス転移温度が低下して耐熱性が悪化するおそれがある。酸無水物の開環率は、ワニスの調製時の加熱温度及び加熱時間により変化する。そのため、開環率が80%以上となるように適宜に加熱条件を調整する。実際に予備反応を行いながら反応物を経時的にサンプリングし、開環率を確認することより、この予備反応の条件を適切に設定することができる。
エポキシ樹脂として、ジシクロペンタジエン型エポキシ樹脂を用いる。具体的には、DIC株式会社製のHP−7200Hを用いる。このエポキシ樹脂のエポキシ当量は、282g/eqである。軟化点は、100℃以上、105℃である。
酸無水物として、新日本理化株式会社製の「リカシッド MH−700」を用いる。この酸無水物は、4−メチルヘキサヒドロ無水フタル酸とヘキサヒドロ無水フタル酸を含み、配合比は、70:30である。また、この酸無水物は、液状脂環式酸無水物である。この酸無水物の酸無水物当量は、161g/eq以上、166g/eq以下である。この酸無水物の酸価は、670KOHmg/gである。
硬化促進剤として、2−エチル−4−メチルイミダゾール(2E4MZ)を用いる。
無機充填材として、破砕シリカを用いる。より具体的には、株式会社アドマテックス製の「MC3000」を用いる。
実施例1〜5、比較例1〜5では、上記のエポキシ樹脂、酸無水物及び硬化促進剤を表1に示す配合量(質量部)で配合する。配合した物を溶媒(MEK)で固形分(非溶媒成分)濃度が60質量%以上、80質量%以下となるように希釈する。これをディスパーで攪拌しながら加熱することによって、エポキシ樹脂と酸無水物の一部とが反応した予備反応生成物を含む1次ワニスを調製する。加熱条件として、温度が60℃以上、80℃以下であり、時間が1時間以上、5時間以下である。この1次ワニスの加熱前後の赤外線吸収スペクトルを測定して、酸無水物の開環率を算出する。その結果、80%以上であった。さらに上記の1次ワニスにSMAを表1に示す配合量(質量部)で配合する。配合した物を攪拌・混合して均一化することにより、ベースワニスを調製する。
上記の樹脂組成物の樹脂ワニスを基材であるガラスクロスに含浸させる。これを非接触タイプの加熱ユニットを用いて110℃以上、140℃以下で加熱乾燥する。樹脂ワニス中の溶媒を除去して、樹脂組成物を半硬化させることによってプリプレグを製造する。ガラスクロスとして、旭化成株式会社製の「1037−AS890AWを用い、重量は23.5g/m2である。プリプレグの樹脂量は、プリプレグ100質量部に対して樹脂組成物72質量部(72質量%)である。プリプレグを加熱および乾燥する際、プリプレグのゲルタイムが140秒以上、160秒以下となるように加熱および乾燥を行う。
金属張積層板は、銅張積層板として製造される。16枚のプリプレグ(340mm×510mm)を重ねて、プリプレグの積層体を構成する。次に、この積層体の厚さ方向の両面に、銅箔を重ねる。そして、銅箔重ねた積層体を加熱および加圧することにより積層成形され金属張積層板が製造される。銅箔には、三井金属鉱業株式会社製の「3EC−III」を用い、厚みは、18μmである。加熱および加圧の条件は、180℃、2.9MPa、60分間である。なお、比較例10のプリプレグと銅箔の密着性は、他のプリプレグと銅箔との密着性と比べて弱く、性能評価できるような金属張積層板を製造することができなかった。これは、酸無水物の揮発により硬化剤が不足して硬化が不十分となったためであると考えられる。
JIS C 6481に準拠して、銅張積層板の表面にける銅箔の引きはがし強さを測定する。すなわち、銅箔を毎分約50mmの速さではがし、そのときの引きはがし強さ(kN/m)をピール強度として測定する。
Hewlett-Packard社製「インピーダンス/マテリアルアナライザー4291A」を用いて、1GHzにおける銅張積層板の比誘電率をIPC−TM−650 2.5.5.9に準じて測定する。
セイコーインスツル株式会社製粘弾性スペクトロメータ「DMS6100」を用いて、プリプレグのガラス転移温度を測定する。具体的には、曲げモジュールで周波数を10Hzとして測定を行い、昇温速度5℃/分の条件で室温から280℃まで昇温した際のtanαが極大を示す温度をガラス転移温度とする。
2 樹脂組成物
3 基材
11 金属張積層板
12,32 絶縁層
13 金属層
14 配線
21 プリント配線板
31 樹脂付き金属箔
エポキシ樹脂として、ジシクロペンタジエン型エポキシ樹脂を用いる。具体的には、DIC株式会社製のHP−7200Hを用いる。このエポキシ樹脂のエポキシ当量は、282g/eqである。軟化点は、100℃以上、105℃以下である。
Claims (7)
- エポキシ樹脂と硬化剤とを有し、
前記硬化剤は、スチレン−無水マレイン酸共重合体と分子中に酸無水物基を一つだけ有した酸無水物とを含み、
前記スチレン−無水マレイン酸共重合体の酸価が300以上、550以下であり、
前記エポキシ樹脂におけるエポキシ基の当量数に対する、前記酸無水物における酸無水物基の当量数の比が0.05以上、0.5以下であり、
前記エポキシ基の当量数に対する、前記酸無水物における酸無水物基の当量数および前記スチレン−無水マレイン酸共重合体における酸無水物基の当量数の合計の比が0.5以上、1.2以下である、
樹脂組成物。 - さらに、前記酸無水物と前記エポキシ樹脂とが反応した予備反応生成物が含有された、
請求項1に記載の樹脂組成物。 - 前記エポキシ樹脂は、ジシクロペンタジエン型エポキシ樹脂を含む、
請求項1又は2に記載の樹脂組成物。 - 請求項1に記載の樹脂組成物と、
前記樹脂組成物が含浸された基材とを有する、
プリプレグ。 - 金属層と、
前記金属層上に設けられた絶縁層とを有し、
前記絶縁層は、請求項1に記載された樹脂組成物の未硬化物を含む、
樹脂付き金属箔。 - 請求項1に記載された樹脂組成物の硬化物を含む絶縁層と、
前記絶縁層上に設けられた金属層とを有する、
金属張積層板。 - 請求項1に記載の樹脂組成物の硬化物を含む絶縁層と、
前記絶縁層上に設けられた配線とを有する、
プリント配線板。
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