JP7359267B2 - 接合用銅ペースト、接合体の製造方法及び半導体装置の製造方法 - Google Patents
接合用銅ペースト、接合体の製造方法及び半導体装置の製造方法 Download PDFInfo
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- JP7359267B2 JP7359267B2 JP2022138060A JP2022138060A JP7359267B2 JP 7359267 B2 JP7359267 B2 JP 7359267B2 JP 2022138060 A JP2022138060 A JP 2022138060A JP 2022138060 A JP2022138060 A JP 2022138060A JP 7359267 B2 JP7359267 B2 JP 7359267B2
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Description
本実施形態の接合用銅ペーストは、金属粒子と、分散媒と、を含む接合用銅ペーストであって、金属粒子がサブマイクロ銅粒子及びマイクロ銅粒子を含む。
本実施形態に係る金属粒子としては、サブマイクロ銅粒子、マイクロ銅粒子、銅粒子以外のその他の金属粒子等が挙げられる。
サブマイクロ銅粒子としては、粒径が0.12μm以上0.8μm以下の銅粒子を含むものが挙げられ、例えば、体積平均粒径が0.12μm以上0.8μm以下の銅粒子を用いることができる。サブマイクロ銅粒子の体積平均粒径が0.12μm以上であれば、サブマイクロ銅粒子の合成コストの抑制、良好な分散性、表面処理剤の使用量の抑制といった効果が得られやすくなる。サブマイクロ銅粒子の体積平均粒径が0.8μm以下であれば、サブマイクロ銅粒子の焼結性が優れるという効果が得られやすくなる。より一層上記効果を奏するという観点から、サブマイクロ銅粒子の体積平均粒径は、0.15μm以上0.8μm以下であってもよく、0.15μm以上0.6μm以下であってもよく、0.2μm以上0.5μm以下であってもよく、0.3μm以上0.45μm以下であってもよい。
マイクロ銅粒子としては、粒径が2μm以上50μm以下の銅粒子を含むものが挙げられ、例えば、体積平均粒径が2μm以上50μm以下の銅粒子を用いることができる。マイクロ銅粒子の体積平均粒径が上記範囲内であれば、接合用銅ペーストを焼結した際の体積収縮を充分に低減でき、接合用銅ペーストを焼結させて製造される接合体の接合強度を確保することが容易となる。接合用銅ペーストを半導体素子の接合に用いる場合、マイクロ銅粒子の体積平均粒径が上記範囲内であれば、半導体装置が良好なダイシェア強度及び接続信頼性を示す傾向にある。より一層上記効果を奏するという観点から、マイクロ銅粒子の体積平均粒径は、3μm以上20μm以下であってもよく、3μm以上10μm以下であってもよい。
金属粒子としては、サブマイクロ銅粒子及びマイクロ銅粒子以外のその他の金属粒子を含んでいてもよく、例えば、ニッケル、銀、金、パラジウム、白金等の粒子を含んでいてもよい。その他の金属粒子は、体積平均粒径が0.01μm以上10μm以下であってもよく、0.01μm以上5μm以下であってもよく、0.05μm以上3μm以下であってもよい。その他の金属粒子を含んでいる場合、その含有量は、充分な接合性を得るという観点から、金属粒子の全質量を基準として、20質量%未満であってもよく、10質量%以下であってもよい。その他の金属粒子は、含まれなくてもよい。その他の金属粒子の形状は、特に限定されるものではない。
分散媒は特に限定されるものではなく、揮発性のものであってもよい。揮発性の分散媒としては、例えば、ペンタノール、ヘキサノール、ヘプタノール、オクタノール、デカノール、エチレングリコール、ジエチレングリコール、プロピレングリコール、ブチレングリコール、α-テルピネオール、イソボルニルシクロヘキサノール(MTPH)等の一価及び多価アルコール類;エチレングリコールブチルエーテル、エチレングリコールフェニルエーテル、ジエチレングリコールメチルエーテル、ジエチレングリコールエチルエーテル、ジエチレングリコールブチルエーテル、ジエチレングリコールイソブチルエーテル、ジエチレングリコールヘキシルエーテル、トリエチレングリコールメチルエーテル、ジエチレングリコールジメチルエーテル、ジエチレングリコールジエチルエーテル、ジエチレングリコールジブチルエーテル、ジエチレングリコールブチルメチルエーテル、ジエチレングリコールイソプロピルメチルエーテル、トリエチレングリコールジメチルエーテル、トリエチレングリコールブチルメチルエーテル、プロピレングリコールプロピルエーテル、ジプロピレングリコールメチルエーテル、ジプロピレングリコールエチルエーテル、ジプロピレングリコールプロピルエーテル、ジプロピレングリコールブチルエーテル、ジプロピレングリコールジメチルエーテル、トリプロピレングリコールメチルエーテル、トリプロピレングリコールジメチルエーテル等のエーテル類;エチレングリコールエチルエーテルアセテート、エチレングリコールブチルエーテルアセテート、ジエチレングリコールエチルエーテルアセテート、ジエチレングリコールブチルエーテルアセテート、ジプロピレングリコールメチルエーテルアセテート(DPMA)、乳酸エチル、乳酸ブチル、γ-ブチロラクトン、炭酸プロピレン等のエステル類;N-メチル-2-ピロリドン、N,N-ジメチルアセトアミド、N,N-ジメチルホルムアミド等の酸アミド;シクロヘキサノン、オクタン、ノナン、デカン、ウンデカン等の脂肪族炭化水素;ベンゼン、トルエン、キシレン等の芳香族炭化水素;炭素数1~18のアルキル基を有するメルカプタン類;炭素数5~7のシクロアルキル基を有するメルカプタン類が挙げられる。炭素数1~18のアルキル基を有するメルカプタン類としては、例えば、エチルメルカプタン、n-プロピルメルカプタン、i-プロピルメルカプタン、n-ブチルメルカプタン、i-ブチルメルカプタン、t-ブチルメルカプタン、ペンチルメルカプタン、ヘキシルメルカプタン及びドデシルメルカプタンが挙げられる。炭素数5~7のシクロアルキル基を有するメルカプタン類としては、例えば、シクロペンチルメルカプタン、シクロヘキシルメルカプタン及びシクロヘプチルメルカプタンが挙げられる。
接合用銅ペーストには、必要に応じて、ノニオン系界面活性剤、フッ素系界面活性剤等の濡れ向上剤;シリコーン油等の消泡剤;無機イオン交換体等のイオントラップ剤などを適宜添加してもよい。
接合用銅ペーストは、上述のサブマイクロ銅粒子、マイクロ銅粒子、その他の金属粒子及び任意の添加剤を分散媒に混合して調製することができる。各成分の混合後に、撹拌処理を行ってもよい。接合用銅ペーストは、分級操作により分散液の最大粒径を調整してもよい。このとき、分散液の最大粒径は20μm以下とすることができ、10μm以下とすることもできる。
以下、図面を参照しながら好適な実施形態について詳細に説明する。なお、図面中、同一又は相当部分には同一符号を付し、重複する説明は省略する。また、図面の寸法比率は、図示の比率に限られるものではない。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.35g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.85gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)3.52gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)5.28gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。密栓をしたポリ瓶を、自転公転型攪拌装置(Planetary Vacuum Mixer ARV-310、株式会社シンキー製)を用いて、2000min-1(2000回転/分)で2分間撹拌した。その後、混合液を超音波ホモジナイザー(US-600、日本精機株式会社製)により19.6kHz、600W、1分間処理した。次いで、密栓したポリ瓶を自転公転型攪拌装置(Planetary Vacuum Mixer ARV-310、株式会社シンキー製)を用いて、2000min-1(2000回転/分)で2分間撹拌した。この混合液を接合用銅ペースト1とした。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.44g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.76gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)4.40gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)4.40gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト2を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.52g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学部式会社製)0.68gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)5.28gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)3.52gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト3を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.61g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン株式会社製)0.59gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)6.16gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)2.64gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト4を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.78g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.42gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)7.91gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)0.88gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト5を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.90gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)6.40gと、マイクロ銅粒子として3L3(福田金属箔粉工業株式会社製)2.75gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト6を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.90gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)4.58gと、マイクロ銅粒子として1110F(三井金属鉱業株式会社製)4.58gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト7を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.61g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.59gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)6.16gと、マイクロ銅粒子としてCu-HWQ3.0μm(福田金属箔粉工業株式会社製)2.64gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト8を調製した。
分散媒としてα-テルピネオール6.1g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.59gと、サブマイクロ銅粒子としてHT-14(表面処理剤不含,三井金属鉱業株式会社製)6.16gと、表面処理剤としてラウリン酸(和光純薬工業株式会社製)0.58gと、を混合し、自動乳鉢で10分混合して混合液を調製した。その後、混合液を超音波ホモジナイザー(US-600、日本精機株式会社製)により19.6kHz、600W、2分間処理し、得られたペースト状組成物をナイロンメッシュ(ボルティングクロス355T、アズワン株式会社製)に通し、HT-14ペースト状組成物を得た。HT-14ペースト状組成物7.36gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)2.64gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト9を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.94g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.26gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)2.64gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)6.16gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト10を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.78g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.42gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)7.92gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)0.88gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト11を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)1.20gと、サブマイクロ銅粒子としてCT-500(表面処理剤:不明、三井金属鉱業株式会社製)7.00gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)3.00gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト12を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)1.20gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)8.80gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト13を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.22g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)1.12gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)0.88gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)7.92gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト14を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)1.20gと、サブマイクロ銅粒子としてCH-0200(表面処理剤:ラウリン酸、三井金属鉱業株式会社製)8.80gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト15を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)1.50gと、銅粒子としてCS-10(表面処理剤:不明、三井金属鉱業株式会社製、50%体積平均粒径:1.1μm、粒径が0.12~0.8μmである粒子の割合(質量%):18%)5.95gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)2.55gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト16を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)1.06gと、銅粒子としてCu-HWQ1.5μm(表面処理剤:なし、福田金属箔粉工業株式会社製、50%体積平均粒径:1.7μm、粒径が0.12~0.8μmである粒子の割合(質量%):11%)6.37gと、マイクロ銅粒子としてMA-C025(三井金属鉱業株式会社製)2.73gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト17を調製した。
分散媒としてα-テルピネオール(和光純薬工業株式会社製)0.67g及びイソボルニルシクロヘキサノール(MTPH、日本テルペン化学株式会社製)0.60gと、マイクロ銅粒子としてCu-HWQ3.0μm(表面処理剤:なし、福田金属箔粉工業株式会社製、50%体積平均粒径:3μm、粒径が0.12~0.8μmである粒子の割合(質量%):0.3%)6.17gと、MA-C025(三井金属鉱業株式会社製)2.64gと、をメノウ乳鉢で乾燥粉がなくなるまで混練し、混合液をポリ瓶に移した。この混合液を用いたこと以外は、調製例1と同様の方法を行い、接合用銅ペースト18を調製した。
(実施例1~7、9~11、16、参考例8)
接合用銅ペースト1~12を用いて、以下の方法に従って接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
19mm×25mmの銅板(厚み:3mm)上に3mm×3mm正方形の開口を3行3列有するステンレス製のメタルマスク(厚さ:100μm)を載せ、メタルスキージを用いたステンシル印刷により接合用銅ペーストを塗布した。塗布した接合用銅ペースト上に、2mm×2mmの被着面がニッケルめっきされた銅ブロック(厚み:250μm)を載せ、ピンセットで軽く押さえた。これをチューブ炉(株式会社エイブイシー製)にセットし、アルゴンガスを3L/minで流して空気をアルゴンガスに置換した。その後、水素ガスを300ml/minで流しながら、10分間昇温した。昇温後、最高到達温度350℃、最高到達温度保持時間10分間の条件で焼結処理して、銅板とニッケルめっきされた銅ブロックとを接合した接合体を得た。焼結後、アルゴンガスを0.3L/minに換えて冷却し、50℃以下で接合体を空気中に取り出した。
接合用銅ペースト4を用いて、以下の方法に従って接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
19mm×25mmの銅板(厚み:3mm)上に3mm×3mm正方形の開口を3行3列有するステンレス製のメタルマスク(厚さ:100μm)を載せ、メタルスキージを用いたステンシル印刷により接合用銅ペーストを塗布した。塗布した接合用銅ペースト上に、2mm×2mmの被着面が金めっきされた銅ブロック(厚み:250μm)を載せ、ピンセットで軽く押さえた。これをチューブ炉(株式会社エイブイシー製)にセットし、アルゴンガスを3L/minで流して空気をアルゴンガスに置換した。その後、水素ガスを300ml/minで流しながら、10分間昇温した。昇温後、最高到達温度350℃、最高到達温度保持時間10分間の条件で焼結処理して、銅板と金めっきされた銅ブロックとを接合した接合体を得た。焼結後、アルゴンガスを0.3L/minに換えて冷却し、50℃以下で接合体を空気中に取り出した。
接合用銅ペースト4を用いて、以下の方法に従って接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
19mm×25mmの銅板(厚み:3mm)上に3mm×3mm正方形の開口を3行3列有するステンレス製のメタルマスク(厚さ:100μm)を載せ、メタルスキージを用いたステンシル印刷により接合用銅ペーストを塗布した。塗布した接合用銅ペースト上に、2mm×2mmの被着面がニッケルめっきされた銅ブロック(厚み:250μm)を載せ、ピンセットで軽く押さえた。この上に15mm×15mmのSUSブロック(重量:15g)を9枚の2mm×2mmの被着面がニッケルめっきされた銅ブロック(厚み:250μm)に重なるように静置し、これをチューブ炉(株式会社エイブイシー製)にセットし、アルゴンガスを3L/minで流して空気をアルゴンガスに置換した。その後、水素ガスを300ml/minで流しながら、10分間昇温した。昇温後、最高到達温度350℃、最高到達温度保持時間10分間の条件で焼結処理して、銅板とニッケルめっきされた銅ブロックとを接合した接合体を得た。焼結後、アルゴンガスを0.3L/minに換えて冷却し、50℃以下で接合体を空気中に取り出した。
接合用銅ペースト4を用いて、以下の方法に従って接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
19mm×25mmの銅板(厚み:3mm)上に3mm×3mm正方形の開口を3行3列有するステンレス製のメタルマスク(厚さ:100μm)を載せ、メタルスキージを用いたステンシル印刷により接合用銅ペーストを塗布した。塗布した接合用銅ペースト上に、2mm×2mmの被着面がニッケルめっきされた銅ブロック(厚み:250μm)を載せ、これをチューブ炉(株式会社エイブイシー製)にセットし、アルゴンガスを3L/minで流して空気をアルゴンガスに置換した。その後、水素ガスを300ml/minで流しながら、10分間昇温した。昇温後、最高到達温度250℃、最高到達温度保持時間60分の条件で焼結処理して、銅板とニッケルめっきされた銅ブロックとを接合した接合体を得た。焼結後、アルゴンガスを0.3L/minに換えて冷却し、50℃以下で接合体を空気中に取り出した。
接合用銅ペースト4を用いて、以下の方法に従って接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
19mm×25mmの銅板(厚み:3mm)上に3mm×3mm正方形の開口を3行3列有するステンレス製のメタルマスク(厚さ:100μm)を載せ、メタルスキージを用いたステンシル印刷により接合用銅ペーストを塗布した。塗布した接合用銅ペースト上に、2mm×2mmの被着面がニッケルめっきされた銅ブロック(厚み:250μm)を載せ、これをチューブ炉(株式会社エイブイシー製)にセットし、アルゴンガスを3L/minで流して空気をアルゴンガスに置換した。その後、水素ガスを300ml/minで流しながら、20分間昇温した。昇温後、最高到達温度450℃、最高到達温度保持時間10分間の条件で焼結処理して銅板とニッケルめっきされた銅ブロックとを接合した接合体を得た。焼結後、アルゴンガスを0.3L/minに換えて冷却し、50℃以下で接合体を空気中に取り出した。
接合用銅ペースト13~18を用いたこと以外は、実施例1と同様の方法により、接合体を製造した。接合体のダイシェア強度は、後述する方法により測定した。
(ダイシェア強度)
接合体の接合強度は、ダイシェア強度により評価した。接合体を、DS-100ロードセルを装着した万能型ボンドテスタ(4000シリーズ、DAGE社製)を用い、測定スピード5mm/min、測定高さ50μmで銅ブロックを水平方向に押し、接合体のダイシェア強度を測定した。8個の接合体を測定した値の平均値をダイシェア強度とした。
島津ナノ粒子径分布測定装置(SALD-7500nano、株式会社島津製作所製)と付属のソフトウェア(WingSALDII-7500- for Japanese V3.、株式会社島津製作所製)を用いて、以下の(1)~(5)に従って50%体積平均粒径を測定した。
(1)ソフトウェアの設定
測定装置付属のパソコンでWingSALDII-7500- for Japanese V3.1を起動し、マニュアルを押し装置の初期化を行った。初期化が終わった後に、保存ファイル名を指定し「次へ」をクリックし、測定条件及び粒子径分布計算条件を以下のように設定し、「次へ」をクリックした。
(測定条件)
・回折/散乱光の検出
平均回数(測定回数:1):128、測定回数:1、測定間隔(秒):2
・測定吸光範囲
最大値:0.2、最小値:0
・ブランク領域/測定領域
ブランク測定許容変動最大値:150、測定最適範囲(MAX):45000、測定最適範囲(MIN):15000
(粒子径分布計算条件)
屈折率の選択:参照試料/順金属/半導体など(固体値)
サンプルの物質:4 Copper(銅)
屈折率の選択:1.18-2.21、「側方/後方センサを評価する」にチェックを入れた
(2)ブランク測定
島津ナノ粒子径分布測定装置SALD-7500nano用回分セル(SALD-BC75、株式会社島津製作所製)をSALD-7500nanoに取り付けて測定を行った。SALD-BC75に付属のロート付き回分セル(部品番号S347-61030-41、株式会社島津製作所製、以下「回分セル」という。)内にα-テルピネオール(和光純薬工業株式会社製)を回分セルの2つの標線の間に収まるようにスポイトで滴下した。WingSALDII-7500- for Japanese V3.の画面上から「診断」、「調整」を選択し、位置センサー出力が装置許容範囲内であることを確認した。「キャンセル」をクリックし元の画面に戻り、ブランク測定を選択し測定を行った。
(3)測定溶液の調製
SALD-BC75に付属の回分セルホルダ(部品番号S347-62301、株式会社島津製作所製)のかくはんレバー上に測定したい接合用銅ペーストを2mg載せ、ロート付き回分セルにセットした。次に、WingSALDII-7500- for Japanese V3.の画面上から「スターラ」を選択し、15分間撹拌を行った。
(4)測定
撹拌後、WingSALDII-7500- for Japanese V3.の画面上から「測定」を選択し測定を行った。(1)~(4)の操作を4回繰り返し、4回測定した。
(5)統計
WingSALDII-7500- for Japanese V3.を起動し、「開く」をクリックし、測定したファイルを選択し、WingSALDII-7500- for Japanese V3.の画面上に測定データを表示した。「重ね描き」をクリックし、画面下段に50.000%径を表示し、4回の平均値を50%体積平均粒径とした。
接合体をカップ内にサンプルクリップ(Samplklip I、Buehler社製)で固定し、周囲にエポキシ注形樹脂(エポマウント、リファインテック株式会社製)をサンプル全体が埋まるまで流し込み、真空デシケータ内に静置し、1分間減圧して脱泡した。その後、室温(25℃)下10時間放置してエポキシ注形樹脂を硬化した。ダイヤモンド切断ホイール(11-304、リファインテック株式会社製)をつけたリファインソー・ロー(RCA-005、リファインテック株式会社製)を用い、注形した接合体の観察したい断面付近で切断した。耐水研磨紙(カーボマックペーパー、リファインテック株式会社製)をつけた研磨装置(Refine Polisher Hv、リファインテック株式会社製)で断面を削りシリコンチップにクラックの無い断面を出し、さらに余分な注形樹脂を削りCP(クロスセクションポリッシャ)加工機にかけられるサイズに仕上げた。切削加工したサンプルをCP加工機(IM4000、株式会社日立ハイテクノロジーズ製)で加速電圧6kV、アルゴンガス流量0.07~0.1cm3/min、処理時間2時間の条件でクロスセクションポリッシングを行って断面加工を行った。断面にスパッタ装置(ION SPUTTER、株式会社日立ハイテクノロジーズ製)を用いて白金を10nmの厚みでスパッタしてSEM観察用のサンプルとした。このSEM用サンプルをSEM装置(ESEM XL30、Philips社製)により、接合体の断面を印加電圧10kVで観察した。
Claims (8)
- 金属粒子と、分散媒と、を含む接合用銅ペーストであって、
前記金属粒子が、体積平均粒径が0.2μm以上0.8μm以下であるサブマイクロ銅粒子と、体積平均粒径が2μm以上50μm以下であるマイクロ銅粒子とを含み、
前記サブマイクロ銅粒子の含有量及び前記マイクロ銅粒子の含有量の合計が、前記金属粒子の全質量を基準として、80質量%以上であり、
前記サブマイクロ銅粒子の含有量が、前記サブマイクロ銅粒子の質量及び前記マイクロ銅粒子の質量の合計を基準として、30質量%以上90質量%以下であり、
前記マイクロ銅粒子が、フレーク状であり、
前記マイクロ銅粒子の含有量は、前記金属粒子の全質量を基準として、10質量%以上90質量%以下であり、
前記サブマイクロ銅粒子が表面処理剤で処理されており、下記式で算出される前記表面処理剤の処理量が0.07質量%以上2.1質量%以下である、接合用銅ペースト。
表面処理剤の処理量(質量%)={(n・A p ・M s )/(S S ・N A +n・A p ・M s )}×100%
[式中、nはサブマイクロ銅粒子の表面に付着した分子層数を示し、A p はサブマイクロ銅粒子の比表面積(単位m 2 /g)を示し、M s は表面処理剤の分子量(単位g/mol)を示し、S S は表面処理剤の最小被覆面積(単位m 2 /個)を示し、N A はアボガドロ数を示す。] - 前記表面処理剤が、炭素数8~16の有機酸である、請求項1に記載の接合用銅ペースト。
- 前記表面処理剤が、ラウリン酸である、請求項1に記載の接合用銅ペースト。
- 第一の部材、請求項1~3のいずれか一項に記載の接合用銅ペースト、及び第二の部材がこの順に積層されている積層体を用意し、前記接合用銅ペーストを、0.01MPa以下の圧力を受けた状態で焼結する工程を備える、接合体の製造方法。
- 第一の部材、請求項1~3のいずれか一項に記載の接合用銅ペースト、及び第二の部材がこの順に積層されている積層体を用意し、前記接合用銅ペーストを、0.01MPa以下の圧力を受けた状態で焼結する工程を備え、
前記第一の部材及び前記第二の部材の少なくとも一方が半導体素子である、半導体装置の製造方法。 - 第一の部材と、第二の部材と、前記第一の部材と前記第二の部材とを接合する請求項1~3のいずれか一項に記載の接合用銅ペーストの焼結体と、を備える、接合体。
- 前記第一の部材及び第二の部材の少なくとも一方が、前記焼結体と接する面に、銅、ニッケル、銀、金及びパラジウムからなる群から選択される少なくとも1種の金属を含む、請求項6に記載の接合体。
- 第一の部材と、第二の部材と、前記第一の部材と前記第二の部材とを接合する請求項1~3のいずれか一項に記載の接合用銅ペーストの焼結体と、を備え、
前記第一の部材及び前記第二の部材の少なくとも一方が半導体素子である、半導体装置。
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JP2010018832A (ja) | 2008-07-09 | 2010-01-28 | Nippon Handa Kk | 金属製部材用接合剤、金属製部材接合体の製造方法、金属製部材接合体、および電気回路接続用バンプの製造方法 |
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WO2014129626A1 (ja) | 2013-02-22 | 2014-08-28 | 古河電気工業株式会社 | 接続構造体、及び半導体装置 |
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KR102580090B1 (ko) | 2023-09-18 |
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US10363608B2 (en) | 2019-07-30 |
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