JP6900954B2 - 接着剤組成物 - Google Patents
接着剤組成物 Download PDFInfo
- Publication number
- JP6900954B2 JP6900954B2 JP2018537305A JP2018537305A JP6900954B2 JP 6900954 B2 JP6900954 B2 JP 6900954B2 JP 2018537305 A JP2018537305 A JP 2018537305A JP 2018537305 A JP2018537305 A JP 2018537305A JP 6900954 B2 JP6900954 B2 JP 6900954B2
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- JP
- Japan
- Prior art keywords
- conductive
- conductive particles
- adhesive
- adhesive composition
- film
- Prior art date
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Images
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- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
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- C09J9/02—Electrically-conducting adhesives
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- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
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Description
フェノキシ樹脂(ユニオンカーバイド株式会社製、製品名:PKHC、重量平均分子量:45000)50gを、トルエン(沸点:110.6℃)と酢酸エチル(沸点:77.1℃)との混合溶剤(質量比でトルエン:酢酸エチル=1:1)に溶解して、固形分40質量%のフェノキシ樹脂溶液を得た。このフェノキシ樹脂溶液に、ラジカル重合性物質として、ウレタンアクリレート(根上工業株式会社製、製品名:UN7700)及びリン酸エステルジメタクリレート(共栄社化学株式会社製、製品名:ライトエステルP−2M)と、硬化剤として1,1−ビス(t−ヘキシルパーオキシ)−3,3,5−トリメチルシクロヘキサン(日本油脂株式会社製、製品名:パーヘキサTMH)とを、フェノキシ樹脂:ウレタンアクリレート:リン酸エステルジメタクリレート:硬化剤=10:10:3:2の固形質量比で配合し溶液A1を得た。
ジビニルベンゼン、スチレンモノマー及びブチルメタクリレートの混合溶液に、重合開始剤としてベンゾイルパーオキサイドを投入して、高速で均一撹拌しながら加熱して重合反応を行うことで微粒子分散液を得た。この微粒子分散液をろ過し減圧乾燥することで、微粒子の凝集体であるブロック体を得た。さらに、このブロック体を粉砕することで、それぞれ架橋密度の異なる平均粒子径20μmの核体(樹脂粒子)を作製した。
上記の核体の表面に、パラジウム触媒(ムロマチテクノス株式会社製、製品名:MK−2605)を担持させて、促進剤(ムロマチテクノス株式会社製、製品名:MK−370)にて活性化させた核体を、60℃に加温された、硫酸ニッケル水溶液、次亜燐酸ナトリウム水溶液及び酒石酸ナトリウム水溶液の混合液中に投入して、無電解メッキ前工程を行った。この混合物を20分間撹拌し、水素の発泡が停止するのを確認した。次に、硫酸ニッケル、次亜リン酸ナトリウム、クエン酸ナトリウム及びメッキ安定剤の混合溶液を添加し、pHが安定するまで撹拌し、水素の発泡が停止するまで無電解メッキ後工程を行った。続いて、メッキ液を濾過し、濾過物を水で洗浄した後、80℃の真空乾燥機で乾燥してニッケルメッキされた導電粒子C1(第2の導電粒子)を作製した。
塩化金酸ナトリウムとイオン交換水との混合溶液に、ニッケルメッキされた導電粒子C1を投入して混合した後、チオ硫酸アンモニウム、亜硫酸アンモニウム及びリン酸水素アンモニウムを投入しメッキ液を調製した。得られたメッキ液にヒドロキシルアミンを投入後、アンモニアを用いてpHを10に調整し、浴温を65℃にして、20分間程度反応させることにより、最外殻が金メッキされた(最外層が金層である)導電粒子C2(第2の導電粒子)を作製した。
テトラクロロパラジウム、エチレンジアミン、アミノピリジン、次亜リン酸ナトリウム、ポリエチレングリコール及びイオン交換水を含む混合溶液中に、ニッケルメッキされた導電粒子C1を投入して混合した後、アンモニアを用いてpHを7.5に調整し、浴温を60℃にして、20分間程度反応させることにより、最外層がパラジウムメッキされた(最外層がパラジウム層である)導電粒子C3(第2の導電粒子)を作製した。
<接着剤組成物のフィルム化>
100体積部の溶液A1に対して、45体積部の導電粒子B1及び15体積部の導電粒子C1を分散させて、混合溶液を得た。得られた混合溶液を、厚み80μmのフッ素樹脂フィルム上に塗布し、70℃で10分間熱風乾燥することにより溶剤を除去して、フッ素樹脂フィルム上に形成された厚み25μmのフィルム状の接着剤組成物を得た。
図4(a),(b)に示すように、得られたフィルム状の接着剤組成物を6mm×6mmに切り出した接着剤フィルム31を、6mm×50mmの銅箔32の略中央に配置し、株式会社大橋製作所製BD−07を用いて加熱加圧(50℃、0.1MPa、2秒間)を行って貼り付けた。続いて、図4(c),(d)に示すように、50mm×6mmのアルミ箔33を用意し、銅箔32と接着剤フィルム31との積層体に対して接着剤フィルム31を覆うように重ねて、株式会社大橋製作所製BD−07で加熱加圧(150℃、0.1MPa、10秒間)を行って、低圧接続時の導電性の評価用の実装体を得た。得られた実装体に対して、図5に示すように電流計、電圧計を接続し、4端子法で接続抵抗(初期)を測定した。結果を表1に示す。
まず、上記の<低圧接続時の導電性の評価>と同様の手順で実装体を作製する場合に、得られる実装体について<低圧接続時の導電性の評価>と同様に測定した接続抵抗(初期)が0.20Ωとなるのに必要な圧力(銅箔32と接着剤フィルム31との積層体に対して接着剤フィルム31を重ねて加熱加圧する際の圧力)P(MPa)を算出した。
次いで、接着剤成分の流出量を、以下に示す手順で評価した。すなわち、上記で得られたフィルム状の接着剤組成物をフッ素樹脂フィルムごと3mm×3mmの正方形に切り取ってフッ素樹脂フィルム付き接着剤フィルムを得た。フッ素樹脂フィルム付き接着剤フィルムの接着剤フィルム面を松浪硝子製角カバーグラス(品番C018181)と接するようにカバーグラス上の略中央に置き、株式会社大橋製作所製BD−07で加熱加圧(60℃、0.1MPa、2秒間)後、フッ素樹脂フィルムを剥がした。続いて、接着剤フィルムの上に更にもう一枚同じカバーグラスを置き、株式会社大橋製作所製BD−07で加熱加圧(130℃、上記で算出した圧力P(MPa)、10秒間)した。スキャナー及びPhotoshop(登録商標)を使用して剥がしたフッ素樹脂フィルムの面積[A]と、加熱加圧後の接着剤フィルムの面積[B]とをピクセル数として測定し、下記式に従って流出量を算出した。結果を表1に示す。
流出量(%)=([B]/[A])×100
図4(a),(b)に示すように、得られたフィルム状の接着剤組成物を6mm×6mmに切り出した接着剤フィルム31を、6mm×50mmの銅箔32の略中央に配置し、株式会社大橋製作所製BD−07を用いて加熱加圧(50℃、0.5MPa、2秒間)を行って貼り付けた。続いて、図4(c),(d)に示すように、50mm×6mmのアルミ箔33を用意し、銅箔32と接着剤フィルム31との積層体に対して接着剤フィルム31を覆うように重ねて、株式会社大橋製作所製BD−07で加熱加圧(150℃、0.5MPa、10秒間)を行って、信頼性の評価用の実装体を得た。
得られた実装体に対して、図5に示すように電流計、電圧計を接続し、4端子法で接続抵抗(初期)を測定した。また、エスペック株式会社製TSA−43ELを使用して、−20℃で30分間保持、10分間かけて100℃まで昇温、100℃で30分間保持、10分間かけて−20℃まで降温、というヒートサイクルを500回繰り返すヒートサイクル試験を実装体に対して行った後に、上記と同様にして接続抵抗(ヒートサイクル試験後)を測定した。ヒートサイクル試験後の接続抵抗が0.5Ω以下であれば、信頼性が良好であると判断した。結果を表1に示す。
接着剤組成物の組成を表1,2に示すとおりに変更した以外は、実施例1と同様にして接着剤組成物を調製し、低圧接続時の導電性、接着剤成分の流出抑制及び信頼性を評価した。結果を表1,2に示す。
Claims (6)
- 電子部材同士の接続に用いられる接着剤組成物であって、
前記電子部材における電極の表面に形成される酸化被膜を貫通可能な突起部を有する導電粒子である第1の導電粒子と、
前記第1の導電粒子以外の導電粒子であって、非導電性の核体及び該核体上に設けられた導電層を有する導電粒子である第2の導電粒子と、
を含有し、
前記導電層が、金又はパラジウムを含有する、接着剤組成物。 - 尖形状の突起部を有する導電粒子である第1の導電粒子と、
前記第1の導電粒子以外の導電粒子であって、非導電性の核体及び該核体上に設けられた導電層を有する導電粒子である第2の導電粒子と、
を含有し、
前記導電層が、金又はパラジウムを含有する、接着剤組成物。 - 前記第1の導電粒子が、異方的な形状を有する導電粒子である、請求項1又は2に記載の接着剤組成物。
- 前記第1の導電粒子が、デンドライト状の導電粒子である、請求項1〜3のいずれか一項に記載の接着剤組成物。
- 前記第1の導電粒子が、フレーク状の導電粒子である、請求項1〜3のいずれか一項に記載の接着剤組成物。
- 前記第2の導電粒子が、略球状の導電粒子である、請求項1〜5のいずれか一項に記載の接着剤組成物。
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CN110783728A (zh) * | 2018-11-09 | 2020-02-11 | 广州方邦电子股份有限公司 | 一种柔性连接器及制作方法 |
US20230002644A1 (en) * | 2019-12-06 | 2023-01-05 | Showa Denko Materials Co., Ltd. | Connector production method and adhesive film |
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TW202214804A (zh) * | 2020-07-17 | 2022-04-16 | 日商京都一來電子化學股份有限公司 | 導電性接著劑組成物 |
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US20010028953A1 (en) * | 1998-11-16 | 2001-10-11 | 3M Innovative Properties Company | Adhesive compositions and methods of use |
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TW201821572A (zh) | 2018-06-16 |
KR20220002723A (ko) | 2022-01-06 |
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CN109642130A (zh) | 2019-04-16 |
KR102345942B1 (ko) | 2021-12-30 |
TWI757326B (zh) | 2022-03-11 |
KR20220154853A (ko) | 2022-11-22 |
US20220363958A1 (en) | 2022-11-17 |
WO2018042701A1 (ja) | 2018-03-08 |
CN116144286A (zh) | 2023-05-23 |
KR102649655B1 (ko) | 2024-03-19 |
US20190241770A1 (en) | 2019-08-08 |
TW202219216A (zh) | 2022-05-16 |
CN109642130B (zh) | 2023-05-02 |
US11414573B2 (en) | 2022-08-16 |
WO2018043505A1 (ja) | 2018-03-08 |
KR20190042654A (ko) | 2019-04-24 |
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