JP2013231097A - 回路接続材料、フィルム状回路接続材料、回路接続シート、回路接続体及び回路部材の接続方法 - Google Patents
回路接続材料、フィルム状回路接続材料、回路接続シート、回路接続体及び回路部材の接続方法 Download PDFInfo
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- JP2013231097A JP2013231097A JP2012102492A JP2012102492A JP2013231097A JP 2013231097 A JP2013231097 A JP 2013231097A JP 2012102492 A JP2012102492 A JP 2012102492A JP 2012102492 A JP2012102492 A JP 2012102492A JP 2013231097 A JP2013231097 A JP 2013231097A
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- AQHHHDLHHXJYJD-UHFFFAOYSA-N propranolol Chemical compound C1=CC=C2C(OCC(O)CNC(C)C)=CC=CC2=C1 AQHHHDLHHXJYJD-UHFFFAOYSA-N 0.000 description 1
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Images
Landscapes
- Polymerisation Methods In General (AREA)
- Graft Or Block Polymers (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Adhesive Tapes (AREA)
Abstract
Description
(測定条件)
装置:東ソー株式会社製 GPC−8020
検出器:東ソー株式会社製 RI−8020
カラム:日立化成工業株式会社製 Gelpack GL−A−160−S+GL−A150
試料濃度:120mg/3ml
溶媒:テトラヒドロフラン
注入量:60μl
圧力:30kgf/cm2
流量:1.00ml/mim
(a)熱可塑性樹脂
ポリエステルウレタン樹脂A
ジカルボン酸としてイソフタル酸(Aldrich社製)を用い、ジオールとしてネオペンチルグリコール(Aldrich社製)を用い、イソシアネートとして4,4’−ジフェニルメタンジイソシアネート(Aldrich社製)を用いて、出発原料におけるイソルタル酸/ネオペンチルグリコール/4,4’−ジフェニルメタンジイソシアネートの質量比が48/37/15であるポリエステルウレタン樹脂Aを合成した。得られたポリエステルウレタン樹脂Aの数平均分子量は25000であり、ガラス転移温度は73℃であった。ポリエステルウレタン樹脂A(PEU―A)を、メチルエチルケトンとトルエンとを1:1(質量比)で混合して調製した混合溶媒に溶解して、濃度40質量%のポリエステルウレタン樹脂溶液を得た。
ジカルボン酸としてテレフタル酸(Aldrich社製)及びアジピン酸(Aldrich社製)を用い、ジオールとしてネオペンチルグリコール(Aldrich社製)を用い、イソシアネートとして4,4’−ジフェニルメタンジイソシアネート(Aldrich社製)を用いて、出発原料におけるテレフタル酸/アジピン酸/ネオペンチルグリコール/4,4’−ジフェニルメタンジイソシアネートのモル比が11/25/38/26であるポリエステルウレタン樹脂Bを合成した。得られたポリエステルウレタン樹脂Bの数平均分子量は40000であり、ガラス転移温度は10℃であった。ポリエステルウレタン樹脂B(PEU―B)を、メチルエチルケトンとトルエンとを0.82:0.18(質量比)で混合して調製した混合溶媒に溶解して、濃度40質量%のポリエステルウレタン樹脂溶液を得た。
ジカルボン酸としてテレフタル酸(Aldrich社製)及びアジピン酸(Aldrich社製)を用い、ジオールとしてネオペンチルグリコール(Aldrich社製)を用い、イソシアネートとして4,4’−ジフェニルメタンジイソシアネート(Aldrich社製)を用いて、出発原料におけるテレフタル酸/アジピン酸/ネオペンチルグリコール/4,4’−ジフェニルメタンジイソシアネートのモル比が34/14/38/14であるポリエステルウレタン樹脂Cを合成した。得られたポリエステルウレタン樹脂Cの数平均分子量は32000であり、ガラス転移温度は18℃であった。ポリエステルウレタン樹脂C(PEU―C)を、メチルエチルケトンとトルエンとを1:1(質量比)で混合して調製した混合溶媒に溶解して、濃度30質量%のポリエステルウレタン樹脂溶液を得た。
フェノキシ樹脂(商品名:YP−50(東都化成株式会社製)、重量平均分子量:60000、ガラス転移温度:80℃)40質量部をメチルエチルケトン60質量部に溶解して、固形分40質量%のフェノキシ樹脂溶液を準備した。
UA1:ウレタンアクリレート1
撹拌機、温度計、塩化カルシウム乾燥管付き還流冷却管、及び窒素ガス導入管を備えた反応容器に、数平均分子量1000のポリ(1,6−ヘキサンジオールカーボネート)(商品名:デュラノール T5652、旭化成ケミカルズ(株)製)2500質量部(2.50モル)と、イソホロンジイソシアネート(シグマ アルドリッチ社製)666質量部(3.00モル)を、3時間かけて均一に滴下した。反応容器内に充分に窒素ガスを導入した後、反応液を70〜75℃に加熱して、反応を進行させた。
撹拌機、温度計、塩化カルシウム乾燥管付き還流冷却管、及び窒素ガス導入管を備えた反応容器に、メチルエチルケトン1000質量部、数平均分子量1000のポリカプロラクトンジオール(商品名:プラクセル210N、ダイセル化学工業(株)製)2500質量部(2.50モル)、及びイソホロンジイソシアネート(シグマ アルドリッチ社製)666質量部(3.00モル)を3時間かけて均一に滴下した。反応容器内に充分に窒素ガスを導入した後、反応液を70〜75℃に加熱して、反応を進行させた。
イソシアヌル酸EO変性ジアクリレート(東亞合成株式会社製)
MAC1
撹拌機、温度計、塩化カルシウム乾燥管付き還流冷却管、及び水分離機を備えた反応容器内で、ヘキサヒドロフタル酸無水物(シグマ アルドリッチ社製)310質量部(2.00モル)をトルエン500質量部に溶解させて、反応液を調製した。反応液を70℃で加熱しながら、エタノールアミン(株式会社日本触媒製)130質量部(2.00モル)を30分かけて滴下し、その後120℃で5時間反応液を攪拌し、生成した水を分離した。冷却後、アクリル酸(シグマ アルドリッチ社製)160質量部(2.20モル)、ハイドロキノンモノメチルエーテル(シグマ アルドリッチ社製)0.2質量部、及び硫酸12質量部を加えて、更に120℃で5時間反応液を攪拌し、生成した水を共沸脱水した。冷却後、分液ロートを用いて反応液を水で洗浄し、さらに残渣のトルエンを減圧蒸留により除去して、下記式(1a)で表される単官能ラジカル重合性化合物(MAC1、N−アクリロイルオキシエチルヘキサヒドロフタルイミド)を得た。
撹拌機、温度計、塩化カルシウム乾燥管付き還流冷却管、及び水分離機を備えた反応容器内で、オルトフェニルフェノール(三光株式会社製)340質量部(2.00モル)をエタノール500質量部に溶解させて、反応液を調製した。反応液を70℃で加熱しながら、硫酸12質量部を30分かけて滴下した。その後、更に120℃で5時間反応液を攪拌し、生成した水を分離した。冷却後、アクリル酸(シグマ アルドリッチ社製)160質量部(2.20モル)、ハイドロキノンモノメチルエーテル(シグマ アルドリッチ社製)0.2質量部、及び硫酸12質量部を加え、更に120℃で5時間反応液を攪拌し、生成した水を共沸脱水した。冷却後、分液ロートを用いて反応液を水で洗浄し、さらに残渣のエタノールを減圧蒸留により除去して、下記式(2a)で表される単官能ラジカル重合性化合物(MAC2、ヒドロキシエチル化o−フェニルフェノールアクリレート)を得た。
ジラウロイルパーオキサイド(パーロイルL、日油株式会社製)
核としてのポリスチレン粒子と、ポリスチレン粒子の表面を覆う厚み0.2μmのニッケル層と、ニッケル層の外側に設けられた厚み0.02μmの金層とから構成される、平均粒径4μm、比重2.5の導電粒子を準備した。
2−メタクリロイロキシエチルホスフェート(商品名:ライトエステル P−2M、共栄社化学(株)製)
コアシェル型シリコーン微粒子(商品名:KMP−600、平均粒径:5μm、信越化学工業(株)製)
表1に示す各成分を表1に示す固形質量比にて配合し、さらに、上記導電粒子を配合しこれを分散させて、各実施例及び比較例の回路接続材料を調製した。導電粒子の量は、回路接続材料全体の体積を基準として1.5体積%とした。得られた各回路接続材料を、厚み80μmのフッ素樹脂フィルム(基材)上に塗工装置を用いて塗布し、塗膜を70℃で10分間熱風乾燥することによって、基材としてのフッ素樹脂フィルム及び基材上に設けられた厚み16μmの接着剤層(フィルム状回路接続材料)を有する接着シートを得た。
ポリイミドフィルム(Tg350℃)及びポリイミドフィルム上に一定方向に並んで設けられた80本の銅回路(ライン幅25μm、ピッチ50μm、厚み8μm)を有するフレキシブル回路板(FPC)と、ガラス基板(厚み1.1mm)及びガラス基板上に形成された厚み0.2μmの酸化インジウム(ITO)薄層からなる回路を有する回路部材(表面抵抗20Ω/□)とを準備し、これらの間に各実施例及び比較例のフィルム状回路接続材料を介在させた。次いで、熱圧着装置(加熱方式:コンスタントヒート型、東レエンジニアリング社製)を用いて、140℃、4MPaで10秒間の加熱及び加圧により、ガラス基板を有する回路部材にFPCを幅3mmにわたり接着して、回路接続体を得た。
Claims (15)
- (a)熱可塑性樹脂と、
(b)2官能以上のラジカル重合性化合物と、
(c)下記一般式(1)又は(2)で表される単官能ラジカル重合性化合物と、
(d)ラジカル重合開始剤と、
を含有する、回路接続材料。
[式(1)中、R1は置換基を有していてもよい芳香族炭化水素基、置換基を有していてもよい脂肪族炭化水素基、置換基を有していてもよい脂環式炭化水素基又はこれらの組み合わせからなる基を示し、R2、R3及びR4はそれぞれ独立に水素原子又は炭素数1〜10のアルキル基を示し、同一分子中の複数のR2及びR4はそれぞれ同一でも異なっていてもよく、nは1〜20の整数を示す。]
[式(2)中、R3及びR4はそれぞれ独立に水素原子又は炭素数1〜10のアルキル基を示し、同一分子中の複数のR4は同一でも異なっていてもよく、R5は置換基を有していてもよい芳香族炭化水素基を示し、nは1〜20の整数を示す。] - 前記熱可塑性樹脂が、ウレタン結合及びエステル結合を有する樹脂を含む、請求項1に記載の回路接続材料。
- 前記熱可塑性樹脂が、60℃以上のガラス転移温度を有する樹脂と、−5℃〜40℃のガラス転移温度を有する樹脂とを含む、請求項1又は2に記載の回路接続材料。
- (f)リン酸基を有し、前記2官能以上のラジカル重合性化合物とは異なるビニル化合物、を更に含有する、請求項1〜3のいずれか一項に記載の回路接続材料。
- (e)導電粒子を更に含有する、請求項1〜4のいずれか一項に記載の回路接続材料。
- フィルム状に成形された請求項1〜5のいずれか一項に記載の回路接続材料からなる、フィルム状回路接続材料。
- 基材と、該基材上に形成された請求項6に記載のフィルム状回路接続材料と、を備える回路接続シート。
- 第一の回路基板及び該第一の回路基板上に設けられた第一の回路電極を有する第一の回路部材と、
第二の回路基板及び該第二の回路基板上に設けられた第二の回路電極を有る第二の回路部材と、
前記第一の回路部材と前記第二の回路部材との間に介在し、前記第一の回路電極と前記第二の回路電極とが電気的に接続されるように前記第一の回路部材と前記第二の回路部材とを接着する接続部と、を備え、
前記接続部が、請求項1〜5のいずれか一項に記載の回路接続材料の硬化物である、回路接続体。 - 前記第一の回路基板及び前記第二の回路基板のうち少なくとも一方が、200℃以下のガラス転移温度を有する熱可塑性樹脂を含む有機基材である、請求項8に記載の回路接続体。
- 前記200℃以下のガラス転移温度を有する熱可塑性樹脂が、ポリエチレンテレフタレート、ポリカーボネート及びポリエチレンナフタレートからなる群より選ばれる少なくとも1種を含む、請求項9に記載の回路接続体。
- 前記第一の回路基板及び前記第二の回路基板のうち少なくとも一方が、ポリエチレンテレフタレート、ポリカーボネート及びポリエチレンナフタレートからなる群より選ばれる少なくとも1種を含む熱可塑性樹脂を含む有機基材である、請求項8に記載の回路接続体。
- 第一の回路基板及び該第一の回路基板上設けられた第一の回路電極を有する第一の回路部材と、第二の回路基板及び該第二の回路基板上に設けられた第二の回路電極を有する第二の回路部材との間に介在する請求項1〜6のいずれか一項に記載の回路接続用材料を硬化させて、前記第一の回路電極と前記第二の回路電極とが電気的に接続されるように前記第一の回路部材と前記第二の回路部材とを接着する工程を備える、回路部材の接続方法。
- 前記第一の回路基板及び前記第二の回路基板のうち少なくとも一方が、200℃以下のガラス転移温度を有する熱可塑性樹脂を含む有機基材である、請求項12に記載の回路部材の接続方法。
- 前記200℃以下のガラス転移温度を有する熱可塑性樹脂が、ポリエチレンテレフタレート、ポリカーボネート及びポリエチレンナフタレートからなる群より選ばれる少なくとも1種を含む、請求項13に記載の回路部材の接続方法。
- 前記第一の回路基板及び前記第二の回路基板のうち少なくとも一方が、ポリエチレンテレフタレート、ポリカーボネート及びポリエチレンナフタレートからなる群より選ばれる少なくとも1種を含む熱可塑性樹脂を含む有機基材である、請求項12に記載の回路部材の接続方法。
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