JP2013216865A - 熱硬化性樹脂充填材及びそれを用いて得られるプリント配線板 - Google Patents
熱硬化性樹脂充填材及びそれを用いて得られるプリント配線板 Download PDFInfo
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- JP2013216865A JP2013216865A JP2013032320A JP2013032320A JP2013216865A JP 2013216865 A JP2013216865 A JP 2013216865A JP 2013032320 A JP2013032320 A JP 2013032320A JP 2013032320 A JP2013032320 A JP 2013032320A JP 2013216865 A JP2013216865 A JP 2013216865A
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- epoxy resin
- mass
- hole
- thermosetting resin
- filler
- Prior art date
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- WHIVNJATOVLWBW-UHFFFAOYSA-N n-butan-2-ylidenehydroxylamine Chemical compound CCC(C)=NO WHIVNJATOVLWBW-UHFFFAOYSA-N 0.000 description 1
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- 229910017464 nitrogen compound Inorganic materials 0.000 description 1
- 150000002830 nitrogen compounds Chemical class 0.000 description 1
- JFOJYGMDZRCSPA-UHFFFAOYSA-J octadecanoate;tin(4+) Chemical compound [Sn+4].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O JFOJYGMDZRCSPA-UHFFFAOYSA-J 0.000 description 1
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- 150000003003 phosphines Chemical class 0.000 description 1
- XYFCBTPGUUZFHI-UHFFFAOYSA-O phosphonium Chemical compound [PH4+] XYFCBTPGUUZFHI-UHFFFAOYSA-O 0.000 description 1
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- IYMSIPPWHNIMGE-UHFFFAOYSA-N silylurea Chemical compound NC(=O)N[SiH3] IYMSIPPWHNIMGE-UHFFFAOYSA-N 0.000 description 1
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Abstract
【解決手段】熱硬化性樹脂充填材は、(A)フェノール型エポキシ樹脂、(B)アミン型エポキシ樹脂、(C)シアネート化合物又はイソシアネート化合物、(D)硬化促進剤、及び(E)無機充填材を含有する。好適には、前記(A)、(B)、(C)成分の配合割合は、エポキシ樹脂全量を100質量部とした場合に、フェノール型エポキシ樹脂は20〜60質量部、アミン型エポキシ樹脂は40〜80質量部であり、さらに上記エポキシ樹脂全量を100質量部とした場合に、シアネート化合物又はイソシアネート化合物が4〜50質量部である。
【選択図】図2
Description
しかしながら、エポキシ樹脂組成物を用いてプリント配線板の永久穴埋め加工を行った場合、加熱硬化時の収縮が大きく、図1に示すように、硬化時にクラックYが発生したり、スルーホール壁との間に隙間が生じるという問題があった。また、エポキシ樹脂組成物の場合、一般に吸水率が大きく、基板の穴埋め部とその上に積層される絶縁層5(プリプレグもしくはソルダーレジスト層)又は樹脂付き銅箔の界面にデラミネーションX(はんだレベリング時にスルーホールの周辺部が浮きあがってしまうという現象、以下、「デラミ」と略称する)が発生するという問題もあった。このようにプリント配線板の穴部に充填された樹脂組成物の硬化物にクラック、デラミ等が発生すると、この部分によって吸湿性を呈し、高温高湿下でのPCT耐性(プレッシャー・クッカー耐性)が低下し、また、プリント配線板のヒートサイクル時のクラック発生や絶縁信頼性の悪化を招いてしまう。さらに、穴部に充填された硬化物の上に形成される絶縁樹脂層や蓋メッキの層間剥離の要因ともなる。
さらに本発明の目的は、絶縁信頼性の悪化、穴部に充填された硬化物の上に形成される絶縁樹脂層や蓋メッキの層間剥離等がなく、絶縁信頼性や耐熱性、低吸水性、保存安定性等の特性に優れる高信頼性のプリント配線板を提供することにある。
(A)フェノール型エポキシ樹脂、
(B)アミン型エポキシ樹脂、
(C)シアネート化合物又はイソシアネート化合物、
(D)硬化促進剤、及び
(E)無機充填材
を含有することを特徴とする熱硬化性樹脂充填材が提供される。
好適な態様においては、エポキシ樹脂全量を100質量部とした場合に、(A)フェノール型エポキシ樹脂は20〜60質量部、(B)アミン型エポキシ樹脂は40〜80質量部であり、さらに上記エポキシ樹脂全量を100質量部とした場合に、(C)シアネート化合物又はイソシアネート化合物が4〜50質量部であることが好ましい。
さらに、本発明の熱硬化性樹脂充填材を用いることにより、プリント配線板のスルーホール、ビアホールなどの穴部に作業性良く充填でき、絶縁信頼性の悪化、穴部に充填された硬化物の上に形成される絶縁樹脂層や蓋メッキの層間剥離等がなく、絶縁信頼性や耐熱性、低吸水性、保存安定性等の特性に優れたプリント配線板を提供できる。
尚、ここでいう「常温」又は「室温」とは、作業環境下での温度範囲と同義であり、例えば一般に約15℃以上、30℃以下の温度範囲に設定される。
上記脂肪酸としては、一般式:(R1COO)n−R2(置換基R1は炭素数が5以上の炭化水素、置換基R2は水素又は金属アルコキシド、金属であり、nが1以上4以下である)で表される化合物を用いることができる。当該脂肪酸は、置換基R1の炭素数が5以上のとき、チキソ性付与の効果を発現させることができる。より好ましくはnが7以上である。脂肪酸としては、炭素鎖中に二重結合あるいは三重結合を有する不飽和脂肪酸であってもよいし、それらを含まない飽和脂肪酸であってもよい。その他、ステアリン酸アルミニウム、ステアリン酸バリウムなどの金属石鹸を用いることもできる。その他の金属石鹸の元素としては、Ca、Zn、Li、Mg,Naなどがある。
表1〜表3に示す成分を、それぞれの配合割合(質量部)にて撹拌機にて予備混合した後、3本ロールミルにて分散を行い、熱硬化性樹脂充填材である実施例1〜15及び比較例1〜6の各ペーストを調製した。
前記のようにして得られた各ペーストについて、以下に列挙するような性能評価を行った。その結果を表4〜表6にまとめて示す。
各ペーストの試料を0.2ml採取し、コーンプレート型粘度計(東機産業社製TV−30)を用いて、25℃、回転数5rpm/minの条件で測定した。
図2に示されるように、パネルめっきにより導体層13が形成されたスルホール12を有する厚さ1.6mm/スルーホール径0.25mm/ピッチ1mmのガラスエポキシ基板11に、実施例及び比較例の各ペーストをスクリーン印刷法により下記印刷条件でスルーホール内に充填した。充填後、熱風循環式乾燥炉に入れ、170℃で60分硬化を行い、評価基板を得た。この評価基板のスルーホール内に充填された硬化物14の充填度合いにより、充填性を評価した。評価基準は以下の通りである。
○:完全に充填されている。
△:一部のスルーホールに充填不良が発生。
×:スルーホールの底部まで充填されていない。
スキージ:スキージ厚20mm、硬度70°、斜め研磨:23°、
版:PET100メッシュバイアス版、
印圧:60kgf/cm2、スキージスピード5cm/Sec、
スキージ角度:80°。
各ペーストの初期と25℃で7日間保管後の粘度の測定を行い、下記の計算式により増粘率を求めた。
増粘率(%)=(初期粘度)/(25℃で7日間保管後の粘度)×100
銅箔の光沢面側に、アプリケーターにて実施例及び比較例で得られた熱硬化性樹脂充填材のペーストを塗布し、170℃で60分硬化させた。硬化後、銅箔から剥離し、硬化皮膜を得た。この硬化皮膜について、誘電率及び誘電正接を以下の条件で測定した。
・測定機器:Agilent Technologies社製E4991A RFインピーダンス・マテリアル・アナライザ。
・測定条件:測定周波数1GHz(n=3で測定)。
予め重量を測定したセラミック板に、実施例及び比較例の熱硬化性樹脂充填材のペーストをスクリーン印刷法で塗布し、熱風循環式乾燥炉にて170℃で60分硬化し、評価サンプルを得た。これを室温まで冷却した後、評価サンプルの重量を測定した。
この評価サンプルを、121℃、100%R.H.、24時間の条件でPCT処理を行い、処理後の硬化物の重量を測定し、下記算式により硬化物の吸水率を求めた。
吸水率(%)=(W2−Wg)/(W1−Wg)×100
ここで、W2はPCT処理後の評価サンプル重量(g)、W1は初期の評価サンプル重量(g)、Wgはセラミック板重量(g)である。
試験基板作製方法:
図2に示されるように、パネルめっきにより導体層13が形成されたスルホール12を有する厚さ1.6mm/スルーホール径0.25mm/ピッチ1mmのガラスエポキシ基板11に、半自動印刷機を用いて実施例及び比較例の熱硬化性樹脂充填材のペーストを充填した。熱風循環式乾燥炉にて170℃で60分硬化後、基板表面からはみ出している硬化物14の部分をバフ研磨により除去した。次いで、PCT(121℃、100%R.H.、24時間)の条件で加湿処理後、前処理としてCZ処理を行った樹脂付き銅箔15(銅箔16にエポキシ樹脂組成物からなる硬化性樹脂17が貼り合わされたもの)をプレス機により積層した。
次いで、最高温度260℃のはんだリフローを5回通し、デラミの有無を確認した。評価基準は以下の通りである。
○:デラミの発生なし。
△:僅かにデラミが確認された。
×:多くのデラミが確認された。
図2に示されるように、パネルめっきにより導体層13が形成されたスルホール12を有する厚さ1.6mm/スルーホール径0.25mm/ピッチ1mmのガラスエポキシ基板11に、半自動印刷機を用いて実施例及び比較例の熱硬化性樹脂充填材のペーストを充填した。熱風循環式乾燥炉にて170℃で60分硬化後、基板表面からはみ出している硬化物14の部分をバフ研磨により除去した。
この評価基板を、288℃のはんだ液中に10秒間、10回浸漬した後、室温まで放冷した。得られた評価基板を目視及び光学顕微鏡で観察し、穴部絶縁層14(スルーホール部内の硬化物)にクラックの発生がないかどうかを確認した。判定基準は以下のとおりである。
○:クラックの発生なし。
△:クラックがわずかに確認された。
×:多くのクラックが確認された。
2、12 スルーホール
3、13 導体層
4、14 穴部絶縁層(熱硬化性樹脂充填材の硬化物)
5 絶縁層
15 樹脂付き銅箔
16 銅箔
X デラミ
Y クラック
Claims (4)
- プリント配線板の凹部及び貫通孔の少なくともいずれか一方に充填するための熱硬化性樹脂充填材であって、
(A)フェノール型エポキシ樹脂、
(B)アミン型エポキシ樹脂、
(C)シアネート化合物又はイソシアネート化合物、
(D)硬化促進剤、及び
(E)無機充填材
を含有することを特徴とする熱硬化性樹脂充填材。 - エポキシ樹脂全量を100質量部とした場合に、(A)フェノール型エポキシ樹脂は20〜60質量部、(B)アミン型エポキシ樹脂は40〜80質量部であり、さらに上記エポキシ樹脂全量を100質量部とした場合に、(C)シアネート化合物又はイソシアネート化合物が4〜50質量部であることを特徴とする請求項1に記載の熱硬化性樹脂充填材。
- 前記(D)硬化促進剤が、金属系硬化促進剤、アミン系硬化促進剤及びイミダゾール系硬化促進剤から選ばれた1種以上であることを特徴とする請求項1又は2に記載の熱硬化性樹脂充填材。
- 前記請求項1〜3のいずれか1項に記載の熱硬化性樹脂充填材の硬化物で充填された穴部を有することを特徴とするプリント配線板。
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Cited By (4)
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JP2015221870A (ja) * | 2014-05-23 | 2015-12-10 | 三菱瓦斯化学株式会社 | プリント配線板材料用樹脂組成物、それを用いたプリプレグ、樹脂シート、金属箔張積層板及びプリント配線板 |
JP2017216398A (ja) * | 2016-06-01 | 2017-12-07 | 凸版印刷株式会社 | ガラス回路基板 |
JP2020182006A (ja) * | 2016-06-01 | 2020-11-05 | 凸版印刷株式会社 | ガラス回路基板 |
WO2022190746A1 (ja) * | 2021-03-08 | 2022-09-15 | 株式会社Adeka | 硬化性樹脂組成物、硬化物及び接着剤 |
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JPH10256687A (ja) * | 1997-03-14 | 1998-09-25 | Matsushita Electric Ind Co Ltd | ビアホール充填用導体ペースト組成物とそれを用いたプリント配線基板 |
JP2001192554A (ja) * | 2000-01-13 | 2001-07-17 | Mitsubishi Gas Chem Co Inc | スルーホール充填用インク及びそれを用いたプリント配線板 |
JP2006028293A (ja) * | 2004-07-14 | 2006-02-02 | Hitachi Chem Co Ltd | 無溶剤1液型の穴埋め用熱硬化性エポキシ樹脂組成物 |
JP2010056274A (ja) * | 2008-08-28 | 2010-03-11 | Sumitomo Bakelite Co Ltd | 多層プリント配線板の製造方法、多層プリント配線板および半導体装置 |
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JPH10256687A (ja) * | 1997-03-14 | 1998-09-25 | Matsushita Electric Ind Co Ltd | ビアホール充填用導体ペースト組成物とそれを用いたプリント配線基板 |
JP2001192554A (ja) * | 2000-01-13 | 2001-07-17 | Mitsubishi Gas Chem Co Inc | スルーホール充填用インク及びそれを用いたプリント配線板 |
JP2006028293A (ja) * | 2004-07-14 | 2006-02-02 | Hitachi Chem Co Ltd | 無溶剤1液型の穴埋め用熱硬化性エポキシ樹脂組成物 |
JP2010056274A (ja) * | 2008-08-28 | 2010-03-11 | Sumitomo Bakelite Co Ltd | 多層プリント配線板の製造方法、多層プリント配線板および半導体装置 |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2015221870A (ja) * | 2014-05-23 | 2015-12-10 | 三菱瓦斯化学株式会社 | プリント配線板材料用樹脂組成物、それを用いたプリプレグ、樹脂シート、金属箔張積層板及びプリント配線板 |
JP2017216398A (ja) * | 2016-06-01 | 2017-12-07 | 凸版印刷株式会社 | ガラス回路基板 |
JP2020182006A (ja) * | 2016-06-01 | 2020-11-05 | 凸版印刷株式会社 | ガラス回路基板 |
WO2022190746A1 (ja) * | 2021-03-08 | 2022-09-15 | 株式会社Adeka | 硬化性樹脂組成物、硬化物及び接着剤 |
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