JPWO2019092960A1 - 焼結接合用組成物、焼結接合用シート、および焼結接合用シート付きダイシングテープ - Google Patents
焼結接合用組成物、焼結接合用シート、および焼結接合用シート付きダイシングテープ Download PDFInfo
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- JPWO2019092960A1 JPWO2019092960A1 JP2019551897A JP2019551897A JPWO2019092960A1 JP WO2019092960 A1 JPWO2019092960 A1 JP WO2019092960A1 JP 2019551897 A JP2019551897 A JP 2019551897A JP 2019551897 A JP2019551897 A JP 2019551897A JP WO2019092960 A1 JPWO2019092960 A1 JP WO2019092960A1
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Abstract
Description
焼結性粒子としての第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)53.78質量部と、焼結性粒子としての第2の銀粒子(平均粒径1100nm,粒径分布400〜5000nm,三井金属鉱業株式会社製)5.976質量部と、熱分解性高分子バインダーとしてのポリカーボネート樹脂(商品名「QPAC40」,重量平均分子量は150000,常温で固体,Empower Materials社製)0.87質量部と、低沸点バインダーとしてのイソボルニルシクロヘキサノール(商品名「テルソルブMTPH」,常温で液体,日本テルペン化学工業株式会社製)3.47質量部と、溶剤としてのメチルエチルケトン 35.91質量部とを、ハイブリッドミキサー(商品名「HM−500」,株式会社キーエンス製)をその撹拌モードで使用して混合し、ワニスを調製した。撹拌時間は3分間とした。そして、得られたワニスを、離型処理フィルム(商品名「MRA50」,三菱樹脂株式会社製)に塗布した後に乾燥させて、焼結接合用の厚さ40μmの粘着層、即ち、焼結接合用組成物の厚さ40μmのシート体を形成した。乾燥温度は110℃とし、乾燥時間は3分間とした。以上のようにして、焼結性粒子と、熱分解性高分子バインダーと、低沸点バインダーとを含む粘着層を有する実施例1の焼結接合用シートを作製した。実施例1の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は93.2質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は90質量%である。このような実施例1の焼結接合用シートに関する組成を表1に掲げる(後記の実施例および比較例についても同様である。また、表1において、組成を表す各数値の単位は、相対的な“質量部”である)。
焼結性粒子としての第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)61.29質量部と、焼結性粒子としての第2の銀粒子(平均粒径1100nm,粒径分布400〜5000nm,三井金属鉱業株式会社製)6.81質量部と、熱分解性高分子バインダーとしてのポリカーボネート樹脂(商品名「QPAC40」,重量平均分子量は150000,常温で固体,Empower Materials社製)0.75質量部と、低沸点バインダーとしてのイソボルニルシクロヘキサノール(商品名「テルソルブMTPH」,常温で液体,日本テルペン化学工業株式会社製)3.02質量部と、溶剤としてのメチルエチルケトン 28.13質量部とを、ハイブリッドミキサー(商品名「HM−500」,株式会社キーエンス製)をその撹拌モードで使用して混合し、ワニスを調製した。撹拌時間は3分間とした。そして、得られたワニスを、離型処理フィルム(商品名「MRA50」,三菱樹脂株式会社製)に塗布した後に乾燥させて、焼結接合用の厚さ40μmの粘着層、即ち、焼結接合用組成物の厚さ40μmのシート体を形成した。乾燥温度は110℃とし、乾燥時間は3分間とした。以上のようにして、焼結性粒子と、熱分解性高分子バインダーと、低沸点バインダーとを含む粘着層を有する実施例2の焼結接合用シートを作製した。実施例2の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は95質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は90質量%である。
第2の銀粒子(平均粒径1100nm,粒径分布400〜5000nm,三井金属鉱業株式会社製)6.81質量部の代わりに第3の銀粒子(平均粒径300nm,粒径分布145〜1700nm,DOWAエレクトロニクス株式会社製)6.81質量部を用いたこと以外は実施例2の焼結接合用シートと同様にして、実施例3の焼結接合用シートを作製した。実施例3の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は95質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は90質量%である。
第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)の配合量を61.29質量部に代えて68.1質量部としたこと、および、第2の銀粒子を用いなかったこと、以外は実施例2の焼結接合用シートと同様にして、実施例4の焼結接合用シートを作製した。実施例4の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は95質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は100質量%である。
第1の銀粒子61.29質量部および第2の銀粒子6.81質量部の代わりに第4の銀粒子(平均粒径20nm,粒径分布1〜50nm,DOWAエレクトロニクス株式会社製)61.29質量部および第5の銀粒子(平均粒径500nm,粒径分布80〜3000nm,三井金属鉱業株式会社製)6.81質量部を用いたこと以外は実施例2の焼結接合用シートと同様にして、実施例5の焼結接合用シートを作製した。実施例5の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は95質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は90質量%である。
第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)の配合量を53.78質量部に代えて35.86質量部としたこと、および、第1および第2の銀粒子に加えて第4の銀粒子(平均粒径20nm,粒径分布1〜50nm,DOWAエレクトロニクス株式会社製)17.93質量部を用いたこと、以外は実施例1の焼結接合用シートと同様にして、実施例6の焼結接合用シートを作製した。実施例6の焼結接合用シート(焼結接合用組成物)における焼結性粒子の含有割合は93.2質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は90質量%である。
第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)の配合量を53.78質量部に代えて35.86質量部としたこと、および、第2の銀粒子(平均粒径1100nm,粒径分布400〜5000nm,三井金属鉱業株式会社製)の配合量を5.976質量部に代えて23.9質量部としたこと、以外は実施例1の焼結接合用シートと同様にして、比較例1の焼結接合用シートを作製した。比較例1の焼結接合用シートにおける焼結性粒子の含有割合は93.2質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は60質量%である。
焼結性粒子としての第1の銀粒子(平均粒径60nm,粒径分布5〜100nm,DOWAエレクトロニクス株式会社製)34.05質量部と、焼結性粒子としての第3の銀粒子(平均粒径300nm,粒径分布145〜1700nm,DOWAエレクトロニクス株式会社製)34.05質量部と、熱分解性高分子バインダーとしてのポリカーボネート樹脂(商品名「QPAC40」,重量平均分子量は150000,常温で固体,Empower Materials社製)0.75質量部と、低沸点バインダーとしてのイソボルニルシクロヘキサノール(商品名「テルソルブMTPH」,常温で液体,日本テルペン化学工業株式会社製)3.02質量部と、溶剤としてのメチルエチルケトン 28.13質量部とを、ハイブリッドミキサー(商品名「HM−500」,株式会社キーエンス製)をその撹拌モードで使用して混合し、ワニスを調製した。撹拌時間は3分間とした。そして、得られたワニスを、離型処理フィルム(商品名「MRA50」,三菱樹脂株式会社製)に塗布した後に乾燥させて、焼結接合用の厚さ40μmの粘着層、即ち、焼結接合用組成物の厚さ40μmのシート体を形成した。乾燥温度は110℃とし、乾燥時間は3分間とした。以上のようにして、焼結性粒子と、熱分解性高分子バインダーと、低沸点バインダーとを含む粘着層を有する比較例2の焼結接合用シートを作製した。比較例2の焼結接合用シートにおける焼結性粒子の含有割合は95質量%であり、当該焼結性粒子における粒径100nm以下の粒子の割合は50質量%である。
実施例1〜6および比較例1,2の各焼結接合用シートを用いて焼結接合を行い、実施例1〜6および比較例1,2の焼結接合用シートごとに、後記の各評価に用いられる必要数のサンプルを作製した。
実施例1〜6および比較例1,2の焼結接合用シートごとに、次のようにして空隙率を調べた。具体的には、まず、冷却環境下において焼結接合用シートについて機械研磨によって断面を露出させた。次に、この露出断面について、イオンポリッシング装置(商品名「クロスセクションポリッシャ SM−09010」,日本電子株式会社製)を使用してイオンポリッシングを行った。次に、当該露出断面における焼結層領域内のSEM像(走査型電子顕微鏡による像)を、電界放出形走査電子顕微鏡SU8020(株式会社日立ハイテクノロジーズ製)を使用して撮像し、反射電子像を画像データとして得た。撮像条件は、加速電圧を5kVとし、倍率を2000倍とした。次に、得られた画像データに対し、画像解析ソフトImageJを使用して、固形部分と空隙部分ないし気孔部分とに2値化する自動2値化処理を施した。そして、当該2値化後の画像から空隙部分の合計面積と全体(固形部分+空隙部分)の面積とを求め、空隙部分の合計面積を全体面積で除して空隙率(%)を算出した。その結果を表1に掲げる。
実施例1〜6および比較例1,2の焼結接合用シートごとに、次のようにして、焼結接合サンプルにおける焼結層の空隙率を調べた。具体的には、まず、機械研磨により、焼結接合サンプルにおいてシリコンチップ対角線に沿った断面を露出させた。次に、この露出断面について、イオンポリッシング装置(商品名「クロスセクションポリッシャ SM−09010」,日本電子株式会社製)を使用してイオンポリッシングを行った。次に、当該露出断面における焼結層領域内のSEM像(走査型電子顕微鏡による像)を、電界放出形走査電子顕微鏡SU8020(株式会社日立ハイテクノロジーズ製)を使用して撮像し、反射電子像を画像データとして得た。撮像条件は、加速電圧を5kVとし、倍率を2000倍とした。次に、得られた画像データに対し、画像解析ソフトImageJを使用して、金属部分と空隙部分ないし気孔部分とに2値化する自動2値化処理を施した。そして、当該2値化後の画像から空隙部分の合計面積と全体(金属部分+空隙部分)の面積とを求め、空隙部分の合計面積を全体面積で除して空隙率(%)を算出した。その結果を表1に掲げる。
実施例1〜6および比較例1,2の焼結接合用シートごとに、次のようにして、焼結接合サンプルにおける焼結層の接合信頼性を調べた。具体的には、まず、冷熱衝撃試験機(商品名「TSE−103ES」,エスペック株式会社製)を使用して、サンプルに対し、−40℃〜200℃の温度範囲での冷熱衝撃を500サイクル与えた。1サイクルの温度プロファイルには、−40℃での15分の保持期間および200℃での15分の保持期間が含まれる。次に、超音波映像装置(商品名「FineSAT II」,日立建機ファインテック株式会社製)を使用して、焼結接合サンプルにおける銅板とシリコンチップとの間の焼結層による接合状態を確認するための撮像を行った。この撮像には、トランスデューサーであるプローブとして、PQ−50−13:WD[周波数50MHz]を使用した。得られた像では、接合状態を維持している領域は灰色で表示され且つ剥離の生じている領域は白色で表示されており、全体面積に対する接合領域総面積の割合を接合率(%)として算出した。その結果を表1に掲げる。
実施例1〜6の焼結接合用シート(焼結接合用組成物)によると、比較例1,2の焼結接合用シートによるよりも、接合対象物間において高密度の焼結層を形成することができ、接合信頼性の高い焼結接合を実現することができた。焼結性粒子の含有割合について、実施例1〜6の焼結接合用シートは比較例1,2の焼結接合用シートと同定度である。また、実施例1〜6の焼結接合用シートに係る焼結接合サンプルの焼結層、および、比較例1,2の焼結接合用シートに係る焼結接合サンプルの焼結層は、加圧力が10MPaであって低負荷の同一焼結条件を経て形成されたものである。そうであるにも関わらず、実施例1〜6の焼結接合用シートによると、比較例1,2の焼結接合用シートによる場合と比較して、有意に空隙率が低くて高密度である焼結層を形成することができ、上記冷熱衝撃試験後の接合率が有意に高い焼結接合を実現することができた。
平均粒径が2μm以下であり、且つ粒径100nm以下の粒子の割合が80質量%以上である、導電性金属含有の焼結性粒子、を含む焼結接合用組成物。
〔付記2〕
前記焼結性粒子の前記平均粒径は、1.5μm以下、1.2μm以下、1μm以下、700nm以下、または500nm以下である、付記1に記載の焼結接合用組成物。
〔付記3〕
前記焼結性粒子の前記平均粒径は70nm以上または100nm以上である、付記1または2に記載の焼結接合用組成物。
〔付記4〕
前記焼結性粒子における粒径100nm以下の粒子の割合は、85質量%以上または90質量%以上である、付記1から3のいずれか一つに記載の焼結接合用組成物。
〔付記5〕
前記焼結性粒子の含有割合が90〜98質量%、92〜98質量%、または94〜98質量%である、付記1から4のいずれか一つに記載の焼結接合用組成物。
〔付記6〕
空隙率が10%以下、8%以下、6%以下、または4%以下である、付記1から5のいずれか一つに記載の焼結接合用組成物。
〔付記7〕
300℃、10MPa、および2.5分間の条件での焼結を経た後の空隙率が10%以下、8%以下、6%以下、または4%以下である、付記1から6のいずれか一つに記載の焼結接合用組成物。
〔付記8〕
熱分解性高分子バインダーを更に含む、付記1から7のいずれか一つに記載の焼結接合用組成物。
〔付記9〕
前記熱分解性高分子バインダーの重量平均分子量は10000以上である、付記8に記載の焼結接合用組成物。
〔付記10〕
前記熱分解性高分子バインダーは、ポリカーボネート樹脂および/またはアクリル樹脂である、付記8または9に記載の焼結接合用組成物。
〔付記11〕
前記焼結性粒子は、銀、銅、酸化銀、および酸化銅からなる群より選択される少なくとも一種を含む、付記1から10のいずれか一つに記載の焼結接合用組成物。
〔付記12〕
70℃での粘度が5×103〜1×107Pa・sまたは1×104〜1×106Pa・sである、付記1から11のいずれか一つに記載の焼結接合用組成物。
〔付記13〕
付記1から12のいずれか一つに記載の焼結接合用組成物のなす粘着層を備える焼結接合用シート。
〔付記14〕
前記粘着層の23℃での厚さは5μm以上または10μm以上である、付記13に記載の焼結接合用シート。
〔付記15〕
前記粘着層の23℃での厚さは100μm以下または80μm以下である、付記13または14に記載の焼結接合用シート。
〔付記16〕
基材と粘着剤層とを含む積層構造を有するダイシングテープと、
前記ダイシングテープにおける前記粘着剤層上の、付記13から15のいずれか一つに記載の焼結接合用シートと、を備える焼結接合用シート付きダイシングテープ。
11 粘着層
12 焼結層
C 半導体チップ
X 焼結接合用シート付きダイシングテープ
20 ダイシングテープ
21 基材
22 粘着剤層
30 半導体ウエハ
Claims (9)
- 平均粒径が2μm以下であり、且つ粒径100nm以下の粒子の割合が80質量%以上である、導電性金属含有の焼結性粒子、を含む焼結接合用組成物。
- 前記焼結性粒子の含有割合が90〜98質量%である、請求項1に記載の焼結接合用組成物。
- 空隙率が10%以下である、請求項1または2に記載の焼結接合用組成物。
- 熱分解性高分子バインダーを更に含む、請求項1から3のいずれか一つに記載の焼結接合用組成物。
- 前記熱分解性高分子バインダーの重量平均分子量は10000以上である、請求項4に記載の焼結接合用組成物。
- 前記熱分解性高分子バインダーは、ポリカーボネート樹脂および/またはアクリル樹脂である、請求項4または5に記載の焼結接合用組成物。
- 前記焼結性粒子は、銀、銅、酸化銀、および酸化銅からなる群より選択される少なくとも一種を含む、請求項1から6のいずれか一つに記載の焼結接合用組成物。
- 請求項1から7のいずれか一つに記載の焼結接合用組成物のなす粘着層を備える焼結接合用シート。
- 基材と粘着剤層とを含む積層構造を有するダイシングテープと、
前記ダイシングテープにおける前記粘着剤層上の、請求項8に記載の焼結接合用シートと、を備える焼結接合用シート付きダイシングテープ。
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