JPWO2008047600A1 - 被覆粒子及びその製造方法、並びに、被覆粒子を用いた異方導電性接着剤組成物及び異方導電性接着剤フィルム - Google Patents
被覆粒子及びその製造方法、並びに、被覆粒子を用いた異方導電性接着剤組成物及び異方導電性接着剤フィルム Download PDFInfo
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Abstract
Description
平均粒径3.5μmの架橋ポリスチレン粒子の表面上に、無電解めっきにより厚み0.2μmのニッケル層を形成した。さらにその形成したニッケル層の外側表面上に、無電解めっきにより厚み0.04μmの金層を形成して導電粒子1を作製した。
<官能基形成工程>
メルカプト酢酸(和光純薬工業株式会社製、商品名)8mmolをメタノール200mlに溶解して導電粒子1を1g加え、直径45mmの攪拌羽を取り付けたスリーワンモーター(新東科学株式会社製、商品名:BL3000)を用いて室温(25℃)で2時間攪拌し、メタノールで洗浄したφ3μmのメンブレンフィルタ(ミリポア社製、商品名:FSLW04700)で濾過して、表面にカルボキシル基を有する官能基含有導電粒子1gを得た。
次に、重量平均分子量70000の30質量%ポリエチレンイミン水溶液(和光純薬工業株式会社製、商品名:30%ポリエチレンイミン P−70溶液)を超純水で希釈して0.3質量%ポリエチレンイミン水溶液を得た。この0.3質量%ポリエチレンイミン水溶液に上記の官能基含有導電粒子1gを加えて室温(25℃)で15分間攪拌し、φ3μmのメンブレンフィルタ(ミリポア社製、商品名:SSWP04700)で濾過して、高分子電解質が表面に吸着した粒子(母粒子)を得た。この母粒子を、超純水200gに混合して室温(25℃)で5分攪拌し、φ3μmのメンブレンフィルタ(ミリポア社製、商品名:SSWP04700)で濾過し、濾過して得られた粒子を該メンブレンフィルタ上で200gの超純水で2回洗浄して、母粒子に吸着していないポリエチレンイミンを除去した。
ポリエチレンイミンを除去後、母粒子1gを、コロイダルシリカ分散液(濃度20質量%、扶桑化学工業社製、商品名:クオートロンPL−13、平均粒子径130nm)を超純水で希釈して得られた0.1質量%シリカ分散液に混合して室温(25℃)で15分間攪拌し、φ3μmのメンブレンフィルタ(ミリポア社製、商品名:SSWP04700)で濾過した。濾過後、母粒子を超純水200gに入れて室温(25℃)で5分攪拌してφ3μmのメンブレンフィルタ(ミリポア社製、商品名:SSWP04700)で濾過し、該メンブレンフィルタ上で母粒子を200gの超純水で2回洗浄して、余剰のシリカを除去した。その後、この母粒子を80℃、30分間の条件で乾燥、次いで120℃、1時間の条件で加熱乾燥して、被覆粒子1を得た。
重量平均分子量70000の30質量%ポリエチレンイミン水溶液の代わりに重量平均分子量10000の30質量%ポリエチレンイミン(和光純薬工業株式会社製、商品名)水溶液を用いたこと以外は、被覆粒子1と同様にして被覆粒子2を得た。
重量平均分子量70000の30質量%ポリエチレンイミン水溶液の代わりに重量平均分子量600の30質量%ポリエチレンイミン(和光純薬工業株式会社製、商品名)水溶液を用いたこと以外は、被覆粒子1と同様にして被覆粒子3を得た。
重量平均分子量70000の30質量%ポリエチレンイミン水溶液を超純水で希釈した0.3質量%ポリエチレンイミン水溶液の代わりに、重量平均分子量100000〜200000の20質量%ポリジアリルジメチルアンモニウムクロリド水溶液(ALDRICH社製、商品名)を超純水で希釈した0.3質量%ポリジアリルジメチルアンモニウムクロリド水溶液を用いたこと以外は、被覆粒子1と同様にして被覆粒子4を得た。
重量平均分子量70000の30質量%ポリエチレンイミン水溶液を超純水で希釈した0.3質量%ポリエチレンイミン水溶液の代わりに、重量平均分子量70000のポリアリルアミン塩酸塩(ALDRICH社製、商品名)を超純水で希釈した0.3質量%ポリアリルアミン塩酸塩水溶液を用いたこと以外は、被覆粒子1と同様にして被覆粒子5を得た。
メルカプト酢酸の代わりに、メルカプト酢酸エチル(和光純薬工業株式会社製、商品名)を用いたこと以外は被覆粒子1と同様にして被覆粒子6を得た。
メルカプト酢酸の代わりに、2−メルカプトエタノール(和光純薬工業株式会社製、商品名)を用いたこと以外は被覆粒子1と同様にして被覆粒子7を得た。
官能基形成工程を実施しなかったこと以外は、被覆粒子1と同様にして被覆粒子8を得た。
高分子電解質吸着工程を実施しなかったこと以外は、被覆粒子1と同様にして被覆粒子9を得た。
フェノキシ樹脂(ユニオンカーバイド社製、商品名:PKHC)100gと、アクリルゴム(ブチルアクリレート40質量部、エチルアクリレート30質量部、アクリロニトリル30質量部、及びグリシジルメタクリレート3質量部の共重合体、重量平均分子量:85万)75gとを酢酸エチル400gに溶解し、ポリマー濃度が30質量%の溶液を得た。この溶液に、マイクロカプセル型潜在性硬化剤を含有する液状エポキシ(エポキシ当量185、旭化成エポキシ株式会社製、商品名:ノバキュアHX−3941)300gを加えて撹拌し、樹脂組成物溶液を作製した。
被覆粒子1の代わりに被覆粒子2を用いたこと以外は、実施例1と同様にして接続体サンプルを得た。
被覆粒子1の代わりに被覆粒子3を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子4を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子5を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子6を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子7を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに導電粒子1を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子8を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
被覆粒子1の代わりに被覆粒子9を用いたこと以外は、実施例1と同様にして接続体サンプルを作製した。
作製した被覆粒子1〜9の表面を走査型電子顕微鏡(PHILIPS製、商品名:XL30 ESEM−FEG)で50000倍に拡大し、0.5μm角のエリア中のシリカ粒子の個数を目視で10点測定し、それらの平均値を求めて単位面積(1μm2)あたりのシリカ被覆量を算出した。シリカ被覆量の算出結果は表1に示すとおりであった。
各実施例及び比較例で用いた被覆粒子を、上述の通り樹脂組成物溶液に混合して分散液を作製した後、分散液2gに対してテトラヒドロフラン30gを入れて、10分間スパチュラで攪拌して樹脂組成物溶液から被覆粒子を抽出した。この被覆粒子を、走査型電子顕微鏡(PHLIPS製、商品名:XL30 ESEM−FEG、倍率25000倍)で観察して被覆粒子からの絶縁性粒子の剥離の有無を確認した。これによって、被覆粒子を樹脂組成物溶液中へ分散させた際の絶縁性粒子の剥離の有無を確認することができる。絶縁性粒子の剥離が殆どないものをOK(剥離無し)、絶縁性粒子が剥離しているものをNG(シリカ剥離)と判定した。抽出試験結果は表1に示す通りであった。
異方導電性接着剤フィルムは互いに隣接するチップ電極間の絶縁抵抗が高く、対向するチップ電極/ガラス電極間の導通抵抗が低いことが重要である。そこで、まず、各実施例及び各比較例で作製した接続体サンプルの絶縁抵抗測定を行った。各実施例及び各比較例の接続体サンプルを各10個作製して、互いに隣接するチップ電極間の絶縁抵抗を測定した。絶縁抵抗の最小値と、絶縁抵抗が109(Ω)を超えるものを良品と判定した場合の歩留まり(良品の割合)とを調べた。絶縁抵抗測定の結果は表1に示す通りであった。
次に、各実施例及び各比較例で作製した接続体サンプルの導通抵抗測定を行った。各実施例及び各比較例の接続体サンプルを各14個作製して、対向する、チップ電極とガラス電極との間の導通抵抗を測定し、その平均値を算出して初期の導通抵抗を求めた。次に、各接続体サンプルを、気温85℃、湿度85%の吸湿条件で1000時間保管した後、対向する、チップ電極とガラス電極との間の導通抵抗を測定し、その平均値を算出して吸湿条件に保管した後(吸湿条件後)の導通抵抗を求めた。導通抵抗測定の結果は表1に示す通りであった。
Claims (16)
- 導電性の金属表面を有し、且つ、該金属表面の少なくとも一部に官能基を有する官能基含有導電粒子の表面の少なくとも一部が、高分子電解質と、表面の少なくとも一部に水酸基を有する無機酸化物からなる絶縁性粒子とを含む絶縁性材料で被覆されてなる被覆粒子。
- 前記官能基は、水酸基、カルボキシル基、アルコキシル基、アルコキシカルボニル基からなる群より選択される少なくとも一つの基である請求項1に記載の被覆粒子。
- 前記官能基は、前記官能基含有導電粒子の金属表面とメルカプト基、スルフィド基、ジスルフィド基からなる群より選択される少なくとも一つの基を有する化合物とを接触させることによって形成されたものである請求項1または2に記載の被覆粒子。
- 少なくとも一部の前記官能基が前記絶縁性粒子の表面の少なくとも一部の前記水酸基と化学結合している請求項1〜3のいずれか一項に記載の被覆粒子。
- 前記高分子電解質がポリアミン類である請求項1〜4のいずれか一項に記載の被覆粒子。
- 前記ポリアミン類がポリエチレンイミンである請求項5に記載の被覆粒子。
- 前記絶縁性粒子がシリカ粒子である請求項1〜6のいずれか一項に記載の被覆粒子。
- 導電粒子の金属表面に、メルカプト基、スルフィド基、ジスルフィド基からなる群より選択される少なくとも一つの基を有する化合物を接触させることにより、前記金属表面の少なくとも一部に官能基を形成して官能基含有導電粒子を得る官能基形成工程と、
前記官能基含有導電粒子の表面の少なくとも一部に、高分子電解質及び表面の少なくとも一部に水酸基を有する無機酸化物からなる絶縁性粒子を接触させる被覆工程と、
を備える、前記官能基含有導電粒子の表面の少なくとも一部が前記高分子電解質と前記絶縁性粒子とを含む絶縁性材料で被覆されてなる被覆粒子の製造方法。 - 前記被覆工程は、前記官能基含有導電粒子の表面の少なくとも一部に前記高分子電解質を接触させた後、前記絶縁性粒子を接触させる工程である請求項8記載の被覆粒子の製造方法。
- 前記官能基は、水酸基、カルボキシル基、アルコキシル基、アルコキシカルボニル基からなる群より選択される少なくとも一つの基である請求項8または9に記載の被覆粒子の製造方法。
- 少なくとも一部の前記官能基が前記絶縁性粒子の表面の少なくとも一部の前記水酸基と化学結合している請求項8〜10のいずれか一項に記載の被覆粒子の製造方法。
- 前記高分子電解質がポリアミン類である請求項8〜11のいずれか一項に記載の被覆粒子の製造方法。
- 前記ポリアミン類がポリエチレンイミンである請求項12に記載の被覆粒子の製造方法。
- 前記絶縁性粒子がシリカ粒子である請求項8〜13のいずれか一項に記載の被覆粒子の製造方法。
- 請求項1〜7のいずれか一項に記載の被覆粒子と、絶縁性の樹脂組成物と、を含有する異方導電性接着剤組成物。
- 請求項15に記載の異方導電性接着剤組成物をフィルム状に形成してなる異方導電性接着剤フィルム。
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JP2008539739A JP4780197B2 (ja) | 2006-10-17 | 2007-10-03 | 被覆粒子及びその製造方法、並びに、被覆粒子を用いた異方導電性接着剤組成物及び異方導電性接着剤フィルム |
PCT/JP2007/069367 WO2008047600A1 (fr) | 2006-10-17 | 2007-10-03 | particule revêtue et son procédé de fabrication, composition adhésive conductrice anisotrope utilisant la particule revêtue et film adhésif conducteur anisotrope |
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CN106688051B (zh) * | 2014-11-20 | 2019-03-29 | 积水化学工业株式会社 | 导电性粒子、导电性粒子的制造方法、导电材料及连接结构体 |
JP6588843B2 (ja) * | 2015-02-19 | 2019-10-09 | 積水化学工業株式会社 | 接続構造体の製造方法 |
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CN101523513A (zh) | 2009-09-02 |
US20100133486A1 (en) | 2010-06-03 |
TW200839793A (en) | 2008-10-01 |
WO2008047600A1 (fr) | 2008-04-24 |
KR101024467B1 (ko) | 2011-03-23 |
EP2079084A4 (en) | 2010-09-08 |
TWI348167B (ja) | 2011-09-01 |
JP4780197B2 (ja) | 2011-09-28 |
EP2079084A1 (en) | 2009-07-15 |
CN101523513B (zh) | 2012-01-11 |
JP4784713B1 (ja) | 2011-10-05 |
JP2011219869A (ja) | 2011-11-04 |
KR20090076974A (ko) | 2009-07-13 |
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