JP5643623B2 - 異方性導電材料及びその製造方法 - Google Patents
異方性導電材料及びその製造方法 Download PDFInfo
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- JP5643623B2 JP5643623B2 JP2010269422A JP2010269422A JP5643623B2 JP 5643623 B2 JP5643623 B2 JP 5643623B2 JP 2010269422 A JP2010269422 A JP 2010269422A JP 2010269422 A JP2010269422 A JP 2010269422A JP 5643623 B2 JP5643623 B2 JP 5643623B2
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- H—ELECTRICITY
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Description
1.異方性導電材料
2.異方性導電材料の製造方法
3.接続方法
4.実施例
本発明の具体例として示す異方性導電材料は、疎水性シリカ表面がジスルフィド系シランカップリング剤で表面処理されたシリカ粒子(以下、スルフィドシラン修飾疎水性シリカという。)を含有するものである。
次に、上述した異方性導電材料の製造方法について説明する。本実施の形態における異方性導電材料の製造方法は、疎水性シリカ表面をジスルフィド系シランカップリング剤で表面処理し、該表面処理されたシリカ粒子を配合するものである。
次に、上述した異方性導電材料を用いた電子部品の接続方法について説明する。本実施の形態における電子部品の接続方法は、第1の電子部品の端子上に上述した異方性導電材料を貼付け、異方性導電フィルム上に第2の電子部品を仮配置させ、第2の電子部品上から加熱押圧装置により押圧し、第1の電子部品の端子と、第2の電子部品の端子とを接続させるものである。
以下、本発明の実施例について説明するが、本発明はこれらの実施例に限定されるものではない。ここでは、実施例1〜6及び比較例1〜7の異方性導電フィルムを作製した。そして、異方性導電フィルムを用いて実装体を作製し、実装体の導通抵抗及び接着強度を評価した。なお、異方性導電フィルムの保存安定性試験、実装体の作製、導通抵抗の測定、及び接着強度の測定は、次のように行った。
実施例3、比較例1及び比較例7の異方性導電フィルムを40℃/60%の環境オーブンに48hr投入した。
実施例1〜6及び比較例1〜7の異方性導電フィルムを用いて、COF(Chip On Film用基材、50μmP、Cu8μmt−Snメッキ、38μmt−S’perflex基材)と、ガラス基板にIZO(Indium Zinc Oxide)膜がコーティングされた厚さ0.7mmのIZOコーティングガラスとを接合し、実装体を完成させた。また、COFと、ガラス基板にSiNx(シリコン窒化)膜がコーティングされた厚さ0.7mmのSiNxコーティングガラスとを接合し、実装体を完成させた。
各実装体について、プレッシャークッカー試験(PCT)を行って接続抵抗値を評価した。初期及び85℃/85%/500hr投入後の接続抵抗値は、デジタルマルチメータ(デジタルマルチメータ7555、横河電機社製)を用いて測定した。測定は、4端子法を用い、電流1mAを流して行った。
各実装体について、プレッシャークッカー試験(PCT)を行って接着強度を評価した。初期及び85℃/85%/500hr投入後の接着強度は、引張試験機(RTC1201、AMD社製)を用いて測定した。測定は、90℃の温度において50mm/secの速度でCOFを引き上げて行った。
(スルフィドシラン修飾疎水性シリカAの作製)
メチルエチルケトン100重量部にビス(3−(エトキシシリル)プロピル)ジスルフィド(商品名:KBE846、信越化学工業社製)を5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、疎水性シリカとして、平均粒径14nmのジメチルシロキサン修飾のシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、スルフィドシラン修飾疎水性シリカAを得た。
膜形成樹脂としてフェノキシ樹脂(商品名:PKHC、巴工業社製)を42質量部、ラジカル重合性物質としてエポキアクリレート(商品名:EB600、ダイセル・サイテック(株)製)を40質量部、ラジカル重合開始剤としてパーオキシケタール(商品名:パーヘキサC、日本油脂(株)製)を3質量部、及びスルフィドシラン修飾疎水性シリカAを15質量部配合して接着剤組成物を得た。この接着剤組成物中に導電性粒子(商品名:AUL704、積水化学工業(株)製)を粒子密度が5000個/mm2になるように分散させ、異方性導電材料を得た。そして、異方性導電材料をPETフィルムに塗布・乾燥させることにより、厚さ20μmの異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は4.5Ω、85℃/85%/500hr投入後の抵抗は7.2Ωであった。
(異方性導電フィルムの作製)
フェノキシ樹脂(商品名:PKHC、巴工業社製)を46質量部、及びスルフィドシラン修飾疎水性シリカAを11質量部とした以外は、実施例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は3.8Ω、85℃/85%/500hr投入後の抵抗は5.6Ωであった。
(異方性導電フィルムの作製)
フェノキシ樹脂(商品名:PKHC、巴工業社製)を49質量部、及びスルフィドシラン修飾疎水性シリカAを8質量部とした以外は、実施例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は3.0Ω、85℃/85%/500hr投入後の抵抗は4.7Ωであった。
(異方性導電フィルムの作製)
フェノキシ樹脂(商品名:PKHC、巴工業社製)を52質量部、及びスルフィドシラン修飾疎水性シリカAを5質量部とした以外は、実施例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は2.6Ω、85℃/85%/500hr投入後の抵抗は4.2Ωであった。
(異方性導電フィルムの作製)
フェノキシ樹脂(商品名:PKHC、巴工業社製)を55質量部、及びスルフィドシラン修飾疎水性シリカAを2質量部とした以外は、実施例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は2.5Ω、85℃/85%/500hr投入後の抵抗は4.3Ωであった。
(スルフィドシラン修飾疎水性シリカBの作製)
メチルエチルケトン100重量部にビス(3−(エトキシシリル)プロピル)ジスルフィド(商品名:KBE846、信越化学工業社製)を2.5質量部及び非スルフィド系シランカップリング剤(商品名:KBM−503、信越化学工業社製)を2.5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、疎水性シリカとして、平均粒径14nmのジメチルシロキサン修飾のシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、スルフィドシラン修飾疎水性シリカBを得た。
膜形成樹脂としてフェノキシ樹脂(商品名:PKHC、巴工業社製)を49質量部、ラジカル重合性物質としてエポキアクリレート(商品名:EB600、ダイセル・サイテック(株)製)を40質量部、ラジカル重合開始剤としてパーオキシケタール(商品名:パーヘキサC、日本油脂(株)製)を3質量部、及びスルフィドシラン修飾疎水性シリカBを8質量部配合して接着剤組成物を得た。この接着剤組成物中に導電性粒子(商品名:AUL704、積水化学工業(株)製)を粒子密度が5000個/mm2になるように分散させ、異方性導電材料を得た。そして、異方性導電材料をPETフィルムに塗布・乾燥させることにより、厚さ20μmの異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は3.1Ω、85℃/85%/500hr投入後の抵抗は4.7Ωであった。
(スルフィドシラン修飾親水性シリカCの作製)
メチルエチルケトン100重量部にビス(3−(エトキシシリル)プロピル)ジスルフィド(商品名:KBE846、信越化学工業社製)を5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、親水性シリカとして、平均粒径14nmのシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、スルフィドシラン修飾親水性シリカCを得た。
膜形成樹脂としてフェノキシ樹脂(商品名:PKHC、巴工業社製)を49質量部、ラジカル重合性物質としてエポキアクリレート(商品名:EB600、ダイセル・サイテック(株)製)を40質量部、ラジカル重合開始剤としてパーオキシケタール(商品名:パーヘキサC、日本油脂(株)製)を3質量部、及びスルフィドシラン修飾親水性シリカCを8質量部配合して接着剤組成物を得た。この接着剤組成物中に導電性粒子(商品名:AUL704、積水化学工業(株)製)を粒子密度が5000個/mm2になるように分散させ、異方性導電材料を得た。そして、異方性導電材料をPETフィルムに塗布・乾燥させることにより、厚さ20μmの異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は6.3Ω、85℃/85%/500hr投入後の抵抗は9.3Ωであった。
(非スルフィドシラン修飾疎水性シリカDの作製)
メチルエチルケトン100重量部にジスルフィド結合を有しないが硫黄を含有するシランカップリング剤(商品名:A−189、モンティブ・パフォーマンス・マテリアルズ社製)を5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、疎水性シリカとして、平均粒径14nmのジメチルシロキサン修飾のシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、非スルフィドシラン修飾疎水性シリカDを得た。
スルフィドシラン修飾親水性シリカCの代わりに、非スルフィドシラン修飾疎水性シリカDを用いた以外は、比較例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は3.1Ω、85℃/85%/500hr投入後の抵抗は5.0Ωであった。
(スルフィドシラン修飾親水性シリカEの作製)
メチルエチルケトン100重量部にジスルフィド結合を有しないが硫黄を含有するシランカップリング剤(商品名:A−189、モンティブ・パフォーマンス・マテリアルズ社製)を5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、親水性シリカとして、平均粒径14nmのシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、スルフィドシラン修飾親水性シリカEを得た。
スルフィドシラン修飾親水性シリカCの代わりに、スルフィドシラン修飾親水性シリカEを用いた以外は、比較例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は8.3Ω、85℃/85%/500hr投入後の抵抗は11.3Ωであった。
(非スルフィドシラン修飾親水性シリカFの作製)
メチルエチルケトン100重量部に非スルフィド系シランカップリング剤(商品名:KBM−503、信越化学工業社製)を5質量部溶解させて処理液を調製した。次いで、この処理液105重量部に、親水性シリカとして、平均粒径14nmのシリカ粒子を10質量部加えて、70℃−2時間静置した後、ろ過し、シリカ粒子を回収し、真空乾燥を行い、非スルフィドシラン修飾親水性シリカFを得た。
スルフィドシラン修飾親水性シリカCの代わりに、非スルフィドシラン修飾親水性シリカFを用いた以外は、比較例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は7.2Ω、85℃/85%/500hr投入後の抵抗は10.7Ωであった。
(親水性シリカG)
平均粒径14nmの親水性シリカGを用いた。
スルフィドシラン修飾親水性シリカCの代わりに、親水性シリカGを用いた以外は、比較例1と同様にして異方性導電フィルムを作製した。なお、シランカップリング剤は配合しなかった。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は8.6Ω、85℃/85%/500hr投入後の抵抗は12.3Ωであった。
(疎水性シリカH)
平均粒径14nmのジメチルシロキサン修飾の疎水性シリカHを用いた。
スルフィドシラン修飾親水性シリカCの代わりに、疎水性シリカHを用いた以外は、比較例1と同様にして異方性導電フィルムを作製した。なお、シランカップリング剤は配合しなかった。
(異方性導電フィルムの作製)
スルフィドシラン修飾親水性シリカCを配合せず、ビス(3−(エトキシシリル)プロピル)ジスルフィド(商品名:KBE846、信越化学工業社製)を8質量部配合した以外は、比較例1と同様にして異方性導電フィルムを作製した。
COFとIZOコーティングガラスとが接合した実装体の導通抵抗を測定したところ、初期抵抗は2.6Ω、85℃/85%/500hr投入後の抵抗は4.3Ωであった。
Claims (7)
- 疎水性シリカ表面がジスルフィド系シランカップリング剤で表面処理されたシリカ粒子を、異方性導電材料100質量部に対して2〜15質量部含有する異方性導電材料。
- 前記ジスルフィド系シランカップリング剤は、スルフィドシランを含む請求項1記載の異方性導電材料。
- 前記疎水性シリカは、シリカ表面をジメチルシロキサンで修飾したジメチルシロキサン修飾シリカである請求項1又は2記載の異方性導電材料。
- 膜形成樹脂と、ラジカル重合性物質と、硬化剤と、導電性粒子とをさらに含有する請求項1〜3のいずれか1項に記載の異方性導電材料。
- 疎水性シリカ表面をジスルフィド系シランカップリング剤で表面処理し、該表面処理されたシリカ粒子を、異方性導電材料100質量部に対して2〜15質量部で配合する異方性導電材料の製造方法。
- 第1の電子部品の端子上に請求項1乃至4のいずれか1項に記載の異方性導電材料を貼付け、
前記異方性導電材料上に第2の電子部品を仮配置させ、
前記第2の電子部品上から加熱押圧装置により押圧し、
前記第1の電子部品の端子と、前記第2の電子部品の端子とを接続させる接続方法。 - 請求項6記載の接続方法により製造される接合体。
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US11437162B2 (en) | 2019-12-31 | 2022-09-06 | Industrial Technology Research Institute | Conductive material composition and conductive material prepared therefrom |
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CN104321279B (zh) * | 2011-11-11 | 2016-09-28 | 维络斯弗洛有限责任公司 | 用于化学附着和变色的多官能超疏水性硅藻土 |
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US9253911B2 (en) | 2016-02-02 |
US20130135838A1 (en) | 2013-05-30 |
TW201236974A (en) | 2012-09-16 |
CN103003892A (zh) | 2013-03-27 |
KR20130122711A (ko) | 2013-11-08 |
JP2011049186A (ja) | 2011-03-10 |
TWI461360B (zh) | 2014-11-21 |
CN103003892B (zh) | 2016-07-06 |
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