JPWO2012160916A1 - 接着剤組成物、フィルム状接着剤、接着シート及び半導体装置 - Google Patents
接着剤組成物、フィルム状接着剤、接着シート及び半導体装置 Download PDFInfo
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- JPWO2012160916A1 JPWO2012160916A1 JP2013516253A JP2013516253A JPWO2012160916A1 JP WO2012160916 A1 JPWO2012160916 A1 JP WO2012160916A1 JP 2013516253 A JP2013516253 A JP 2013516253A JP 2013516253 A JP2013516253 A JP 2013516253A JP WO2012160916 A1 JPWO2012160916 A1 JP WO2012160916A1
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Abstract
Description
溶媒:ジメチルホルムアミド(DMF)+臭化リチウム(LiBr)(0.03mol(対DMF1L)+りん酸(0.06mol(対DMF1L))
カラム:G6000HXL+G4000HXL+G2000HXL(東ソー株式会社製)試料濃度:10mg/5mL
注入量:0.5mL
圧力:100kgf/cm2
流量:1.00mL/分
測定温度:25℃。
また、上記熱流動温度とは、フィルム化した試料を使用して、レオメトリックス製粘弾性アナライザーRSA−2を用いて、フィルムサイズ35mm×10mm×40μm厚、昇温速度5℃/分、周波数1Hz、測定温度−150〜300℃の条件で測定し、貯蔵弾性率が0.1MPa以下となる温度である。
下記材料を用い、表1に示す組成(質量部)で混合し、実施例1〜3及び比較例1〜6の接着剤層形成用ワニスをそれぞれ調製した。
PU:DIC Bayer Polymer(ディーアイシー バイエル ポリマー)、ポリウレタン樹脂T−8175(Tg:−23℃,重量平均分子量:81000)
ZX−1395:東都化成、ビスフェノールF型フェノキシ樹脂(Tg:68℃、重量平均分子量:88000)
HP−850N:日立化成、フェノールノボラック樹脂(OH当量:106)
TPPK:東京化成、テトラフェニルホスホニウムテトラフェニルボラート
2P4MHZ:四国化成株式会社製、2−フェニル−4−メチル−5−ヒドロキシメチルイミダゾール
BMI−1000:東京化成株式会社製、4,4’−ビスマレイミドジフェニルメタン
パークミルD:日本油脂株式会社製、ジクミルパーオキサイド
UG−4010:東亜合成株式会社製、エポキシ基含有無溶剤型液状アクリルポリマー(ARUFON,Tg:−57℃,重量平均分子量:2900)
HP−P1:水島合金鉄、窒化ホウ素フィラー
NMP:関東化学、N−メチル−2−ピロリドン
温度計、攪拌機、冷却管、及び窒素流入管を装着した300mLフラスコ中に、1,3−ビス(3−アミノプロピル)テトラメチルジシロキサン(信越化学工業株式会社製、商品名:LP−7100)15.53g、ポリオキシプロピレンジアミン(BASF株式会社製、商品名:D400、分子量:450)28.13g、及びNMP100.0gを仕込んで攪拌して、反応液を調製した。ポリオキシプロピレンジアミンが溶解した後、フラスコを氷浴中で冷却しながら、予め無水酢酸からの再結晶により精製した4,4’−オキシジフタル酸二無水物32.30gを反応液に少量ずつ添加した。常温(25℃)で8時間反応させた後、キシレン67.0gを加え、窒素ガスを吹き込みながら180℃で加熱することにより、水と共にキシレンを共沸除去した。その反応液を大量の水中に注ぎ、沈澱した樹脂を濾過により採取し、乾燥してポリイミド樹脂(PI−1)を得た。得られたポリイミド樹脂(PI−1)の分子量をGPCにて測定したところ、ポリスチレン換算で、数平均分子量Mn=21200、重量平均分子量Mw=43400であった。ポリイミド樹脂(PI−1)のTgは45℃であった。
温度計、攪拌機、冷却管、及び窒素流入管を装着した300mLフラスコ中に、2,2−ビス(4−アミノフェノキシフェニル)プロパン13.68g、4,9−ジオキサドデカン−1,12−ジアミン6.80g、及びNMP165.8gを仕込んで攪拌して、反応液を調製した。4,9−ジオキサドデカン−1,12−ジアミンが溶解した後、フラスコを氷浴中で冷却しながら、予め無水酢酸からの再結晶により精製したデカメチレンビストリメリテート二無水物34.80gを反応液に少量ずつ添加した。常温(25℃)で8時間反応させた後、キシレン110.5gを加え、窒素ガスを吹き込みながら180℃で加熱することにより、水と共にキシレンを共沸除去した。その反応液を大量の水中に注ぎ、沈澱した樹脂を濾過により採取し、乾燥してポリイミド樹脂(PI−3)を得た。得られたポリイミド樹脂(PI−2)の分子量をGPCにて測定したところ、ポリスチレン換算で、数平均分子量Mn=28900、重量平均分子量Mw=88600であった。ポリイミド樹脂(PI−2)のTgは67℃であった。
〔成膜性の評価〕
接着シートの作製
実施例1〜3及び比較例1〜6の接着剤層形成用ワニスを、乾燥後の膜厚が40μm±5μmとなるように、それぞれ支持フィルム上に塗布した。支持フィルムとして二軸延伸ポリプロピレン(OPP)フィルム(厚さ60μm)を用いた。塗布された接着剤層形成用ワニスをオーブン中にて80℃で30分間、続いて、120℃で30分間加熱することにより乾燥して、支持フィルム及び該支持フィルム上に形成されたフィルム状の接着剤層を有する接着シートを得た。
上記条件で得られた接着シートについて、以下の基準により成膜性を評価した。下記基準で成膜性の評価がAであるとき、薄膜形成性が優れることを意味する。
A:フィルム状の接着剤層が支持基材上でハジキ(cissing)がなく塗工可能であり、得られた接着シートから支持基材をはく離可能
C:支持基材上でフィルム状の接着剤層のハジキがある(得られたフィルム面積が70%以下に縮小)
接着シートの作製
実施例1〜3及び比較例1〜6の接着剤層形成用ワニスを40μmの厚さに、それぞれ基材(剥離剤処理PET)上に塗布し、オーブン中で、80℃で30分、続いて120℃で30分加熱し、基材及び該基材上に形成されたフィルム状の接着剤層を有する接着シートを得た。
得られた各接着シートから、幅10mm、長さ40mmの試験片を切り出した。この試験片を、支持台上に載せたシリコンウェハ(6インチ径、厚さ400μm)の裏面(支持台と反対側の面)に、接着剤層がシリコンウェハ側になる向きで積層した。積層は、ロール(温度100℃、線圧4kgf/cm、送り速度0.5m/分)で加圧する方法により行った。
A:ピール強度が2N/cm以上
C:ピール強度が2N/cm未満
成膜性の評価と同様の方法により得られた、厚さ60μmのOPP基材上に40μm厚にフィルム状の接着剤層を形成させた接着シートを、10mm×10mmサイズに切断して試験片とした。この試験片を、2枚のスライドグラス(松浪硝子工業株式会社製、76mm×26mm×1.0〜1.2mm厚)の間に挟み、120℃の熱盤上で全体に100kgf/cm2の荷重を加えながら15秒間加熱圧着した。加熱圧着後の上記OPP基材の四辺からのフィルム状接着剤のはみ出し量をそれぞれ光学顕微鏡で計測し、それらの平均値をフロー量とした。Bステージ状態の接着シート及びCステージ状態の接着シートについて、このフロー量を測定した。なお、Bステージとは、接着剤層形成用ワニスをOPP基材上に塗工後、オーブン中にて80℃で30分間、続いて120℃で30分間の条件で加熱した後の状態のことであり、Cステージとはオーブン中で更に180℃で5時間の条件で加熱硬化した後の状態のことである。また、フィルムの厚さは±5μmの誤差で調整した。Bステージでのフロー量が多く、Cステージでのフロー量が少ない程、熱時流動性に優れることを意味する。
成膜性の評価と同様の方法により得られた各接着シートの接着剤層(5mm×5mm×40μm厚)を、42アロイリードフレームと、突起部を有するシリコンチップ(5mm×5mm×400μm厚)との間に介在させ、その状態で加熱圧着した。加熱温度は実施例1〜3、比較例1、3、5及び6では150℃、比較例2及び4では200℃に設定した。加圧は荷重:1kgf/chip、時間:5秒間の条件で行った。加熱圧着後、オーブン中で180℃で5時間加熱して接着剤層を硬化させて、ピール強度測定用のサンプルとしての積層体を得た。
Claims (11)
- ポリウレタン樹脂と熱硬化性成分とを含み、
Bステージでの120℃におけるフロー量が500μm以上であり、かつCステージでの120℃におけるフロー量が500μm未満であり、
前記Bステージでの120℃におけるフロー量を(A)、前記Cステージでの120℃におけるフロー量を(B)としたとき、(A)−(B)の値が100μm以上である接着剤組成物。 - 前記熱硬化性成分がエポキシ樹脂を含む、請求項1に記載の接着剤組成物。
- 前記熱硬化性成分がビスマレイミド樹脂を含む、請求項1に記載の接着剤組成物。
- 更にフィラーを含有する、請求項1〜3のいずれか一項に記載の接着剤組成物。
- 半導体素子同士、又は半導体素子と半導体素子搭載用支持部材との接着用である、請求項1〜4のいずれか一項に記載の接着剤組成物。
- 前記半導体素子搭載用支持部材が、前記半導体素子を搭載する面に配線段差を有する有機基板である、請求項5に記載の接着剤組成物。
- 請求項1〜4のいずれか一項に記載の接着剤組成物をフィルム状に形成してなるフィルム状接着剤。
- 支持基材と、該支持基材の主面上に形成された請求項7に記載のフィルム状接着剤と、を備える接着シート。
- 前記支持基材がダイシングシートである、請求項8に記載の接着シート。
- 前記ダイシングシートが、基材フィルム及び該基材フィルム上に設けられた粘着剤層を有する、請求項9に記載の接着シート。
- 半導体素子と半導体素子搭載用支持部材とが請求項1〜4のいずれか一項に記載の接着剤組成物の硬化物により接続された構造、又は隣接する半導体素子同士が請求項1〜4のいずれか一項に記載の接着剤組成物の硬化物により接続された構造を備える半導体装置。
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JP2021011512A (ja) * | 2019-07-03 | 2021-02-04 | 昭和電工マテリアルズ株式会社 | 接着剤組成物、フィルム状接着剤、接着シート、ダイシング・ダイボンディング一体型接着シート、並びに半導体装置及びその製造方法 |
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