JP7147995B2 - 導電性ピラー、接合構造、電子機器および導電性ピラーの製造方法 - Google Patents
導電性ピラー、接合構造、電子機器および導電性ピラーの製造方法 Download PDFInfo
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- JP7147995B2 JP7147995B2 JP2021554163A JP2021554163A JP7147995B2 JP 7147995 B2 JP7147995 B2 JP 7147995B2 JP 2021554163 A JP2021554163 A JP 2021554163A JP 2021554163 A JP2021554163 A JP 2021554163A JP 7147995 B2 JP7147995 B2 JP 7147995B2
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- conductive pillar
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Description
また、本発明は、本発明の導電性ピラーを有し、基材と被接合部材とを高い接合強度で接合できる接合構造および電子機器を提供することを目的とする。
前記金属微粒子のX線小角散乱測定法を用いて測定した平均粒子径が1μm未満であり、
前記焼結体の上面が、前記基材側に窪んだ凹型形状であることを特徴とする導電性ピラー。
[2] 前記金属微粒子が、AgおよびCuから選択される1種以上の金属であることを特徴とする[1]に記載の導電性ピラー。
基材上に設けられた金属微粒子の焼結体で構成され、前記金属微粒子のX線小角散乱測定法を用いて測定した平均粒子径が1μm未満であり、前記焼結体の上面が、前記基材側に窪んだ凹型形状である導電性ピラーと、
前記導電性ピラーの前記凹部形状に沿って設けられた接合層とを有することを特徴とする接合構造。
[4] 前記導電性ピラーが上面から前記基材に向かって延出する複数の溝部を有し、 前記溝部内に前記接合層の一部が充填されたアンカー部を有することを特徴とする[3]に記載の接合構造。
[6] 前記導電性ピラーと前記接合層との間に、金属間化合物層を有することを特徴とする[3]~[5]のいずれかに記載の接合構造。
前記柱状体を焼結して、上面に前記基材側に窪んだ凹型形状を有する焼結体を形成する工程とを有することを特徴とする導電性ピラーの製造方法。
[11] 前記焼結体を形成する工程の前に、前記柱状体の少なくとも表面を酸素濃度200ppm以上の酸素含有雰囲気に暴露する工程を有することを特徴とする[9]または[10]に記載の導電性ピラーの製造方法。
本発明の電子機器は、本発明の接合構造を含むため、基材と被接合部材とが高い接合強度で接合されたものとなる。
本発明の導電性ピラーの製造方法によれば、電気メッキ法を用いずに、基材と被接合部材とを接合層を介して高い接合強度で接合できる本発明の導電性ピラーを製造できる。
図1は、本実施形態の導電性ピラーの一例を示した側面図である。図2(A)は図1に示した導電性ピラーの平面図である。図2(B)は図2(A)に示した導電性ピラーをA-A´線に沿って切断した断面図である。
本実施形態の導電性ピラー1は、図1に示すように、焼結体12で構成されている。焼結体12は、図1に示すように、電極パッド13を有する基材11上に設けられている。
焼結体12の大きさ(導電性ピラー1の大きさ)は、電子機器の小型化に伴う接合構造の微細化に対応できるように、直径100μm以下であることが好ましく、更に好ましくは50μm以下であり、特に好ましくは30μm以下である。焼結体12の大きさ(導電性ピラー1の大きさ)は、後述する接合層との接合性および導電性がより一層良好なものとなるため、直径5μm以上であることが好ましく、20μm以上であることがより好ましい。
本実施形態においては、焼結体12を形成している金属微粒子の平均粒子径として、X線小角散乱測定法(Small-Angle X-ray Scattering、SAXS)を用いて測定した測定値を用いる。
さらに、導電性ピラー1が平均粒子径1μm未満の金属微粒子の焼結体12であるため、焼結によって得られる金属微粒子同士の融着機能により、導電性ピラー1の形状を形成できる。
次に、本実施形態の導電性ピラーの製造方法について、例を挙げて詳細に説明する。 図3(A)~図3(C)は、図1および図2に示す導電性ピラー1の製造方法の一例を説明するための工程図である。
本実施形態では、図3(A)~図3(C)に示すように、基材11上に3つの導電性ピラー1を形成する場合を例に挙げて説明するが、基板11上に形成する導電性ピラー1の数は、3つに限定されるものではなく、1つまたは2つでもよいし、4つ以上であってもよく、必要に応じて決定される。また、基板11上に形成する複数の導電性ピラー1の配置は、基材11上に設けられた電極パッド13の配置に応じて、適宜決定される。
導電性ペースト12cをレジスト開口部16aに充填する際には、アルゴンガス雰囲気などの不活性ガス雰囲気下または還元性ガス雰囲気下で行ってもよい。この場合、導電性ペースト12cに含まれる金属微粒子が酸化されにくく、好ましい。
導電性ペースト12cをレジスト開口部16aに充填する方法としては、スキージ12dを用いる方法に限定されるものではなく、ドクタープレード、ディスペンサ、インクジェット、プレス注入、真空印刷、加圧による押込みなどの方法を用いてもよい。
本実施形態では、導電性ピラー1の材料として使用される金属微粒子の平均一次粒子径として、TEMを用いて撮影した写真の画像を解析することにより算出した値を用いる。
酢酸銅(II)-水和物と、分散剤としての式(1)で示される化合物と、エチレングリコールとからなる混合物に、窒素を吹き込みながら加熱し、攪拌し、脱気してから室温に戻す。次いで、室温に戻した混合物に、ヒドラジン水和物を水で希釈したヒドラジン溶液を滴下して、銅を還元する。
以上の工程により、銅からなる金属微粒子と、式(1)で示される化合物からなる分散剤との複合体〔1〕が得られる。
硝酸銀(I)と、分散剤としての式(1)で示される化合物と、蒸留水とからなる混合物に、還元剤としてのジメチルアミノエタノールと蒸留水との混合液を滴下する。その後、混合液を加熱して還元反応を終結させる。
以上の工程により、銀からなる金属微粒子と、式(1)で示される化合物からなる分散剤との複合体〔2〕が得られる。
硝酸銅と、保護剤としてのオクチルアミンおよびリノール酸とを、トリメチルペンタンに混合攪拌して溶解し、混合溶液とする。その後、この混合溶液に、水素化ホウ素ナトリウムを含むプロパノール溶液を滴下して銅を還元する。
以上の工程により、黒色の固体からなり、銅からなる金属微粒子と、有機物からなる保護剤との複合体〔3〕が得られる。
アルゴンガス雰囲気下で、保護剤としてのN,N-ジメチルエチレンジアミンおよび3-(2-エチルヘキシルオキシ)プロピルアミンからなる混合液を加熱攪拌し、さらにシュウ酸銀を添加して加熱攪拌して反応させる。
以上の工程により、銀からなる金属微粒子と、有機物からなる保護剤との複合体〔4〕が得られる。
柱状体の少なくとも表面を暴露する酸素含有雰囲気における酸素濃度は、30%以下であることが好ましく、25%以下であることがより好ましく、大気中の酸素濃度(20.1%)以下であることがさらに好ましい。酸素含有雰囲気中の酸素濃度が30%以下であると、柱状体を形成している導電性ペースト12cに含まれる金属微粒子が、過剰に酸化されることを防止できる。
酸素濃度200ppm以上の酸素含有雰囲気としては、例えば、大気が挙げられる。
柱状体を焼成する焼成方法としては、特に限定されるものではなく、例えば、真空はんだリフロー装置、ホットプレート、熱風オーブンなどを用いることができる。
以上の工程により、本実施形態の導電性ピラー1が得られる。
次に、本実施形態の接合構造について詳細に説明する。図4(A)は、本実施形態の接合構造の一例を示した断面図である。図4(A)に示す接合構造20は、上述した本実施形態の導電性ピラー1を有する。
図4(A)に示すように、本実施形態の接合構造20は、基材11と、基材11と対向配置される被接合部材21との間に配置されている。被接合部材21としては、例えば、任意の電気回路が形成され、表面に電極23を有する半導体パッケージなどが挙げられる。
本実施形態の接合構造20は、本実施形態の導電性ピラー1と、導電性ピラー1の凹部形状に沿って設けられた接合層22とを有する。図4(A)に示す接合構造20では、図3(C)に示す導電性ピラー1が、図3(C)における上下方向を反転させた状態で設置されている。
本実施形態においては、接合層22が一種類の材料からなる単層構造である場合を例に挙げて説明するが、接合層は、二種類以上の材料が積層された多層構造のものであってもよい。
接合層22の材料として用いるはんだ合金としては、Sn-Ag合金、Sn-Pb合金、Sn-Bi合金、Sn-Zn合金、Sn-Sb合金、Sn-Bi合金、Sn-In合金、Sn-Cu合金、SnにAu、Ag、Bi、InおよびCuからなる群より選ばれる2つの元素を添加した合金等を用いることができる。
次に、図4(A)に示す本実施形態の接合構造20の製造方法として、図3(C)に示す導電性ピラー1を用いて接合構造を製造する場合を例に挙げて詳細に説明する。
図5(A)~図5(C)は、図4(A)に示す接合構造の製造方法の一例を説明するための工程図である。
本実施形態では、接合層22を形成した後に、レジスト層16を除去する場合を例に挙げて説明したが、レジスト層16は、接合層22の形成後に除去しなくてもよい。レジスト層16を除去しない場合、レジスト層16は、基材11と後述する被接合部材とを積層することにより、基材11と被接合部材との間に配置される。
以上の工程により、図4(A)に示す接合構造20が得られる。
本実施形態では、図4(A)に示すように、基材11と被接合部材21との間に配置された3つの接合構造20が、全て略同じ形状を有する場合を例に挙げて説明したが、基材11と被接合部材21との間に本実施形態の接合構造が複数設けられている場合、複数の接合構造のうち、一部または全部が異なる形状であってもよい。すなわち、各接合構造の有する導電性ピラーおよび接合層の形状は、基材11の電極パッドおよび被接合部材21の電極の平面形状に応じて適宜決定できる。
図4(B)に示すように、基材11と被接合部材21との間には、複数(図4(B)に示す例では3つ)の接合構造20a、20b、20cが設けられている。図4(B)に示す接合構造20a、20b、20cにおいては、3つの接合構造20a、20b、20cのうち1つの接合構造20aの平面形状が、他の接合構造20b、20cよりも大きいものとなっており、他の接合構造20b、20cの形状が同じとなっている。
また、図4(B)においては、3つの接合構造20a、20b、20cにおける基材11の厚み方向の長さが略同じである場合を例に挙げて説明したが、各接合構造の基材11の厚み方向の長さは、一部または全部が異なっていてもよい。
本実施形態の電子機器は、本実施形態の接合構造20を含む。本実施形態の電子機器は、接合構造20を複数含むことが好ましい。この場合、複数の接合構造20のうち、一部または全部が異なる形状であってもよい。
具体的には、本実施形態の電子機器としては、本実施形態の接合構造20を複数含む3次元(3D)実装構造を有するデバイス、または本実施形態の接合構造20を複数含むインターポーザを用いた2.5次元(2.5D)実装構造を有するデバイスなどが挙げられる。
本実施形態の電子機器は、本実施形態の接合構造20を含むため、基材11と被接合部材21とが高い接合強度で接合されたものとなる。
[金属微粒子を含む導電性ペーストの製造]
導電性ピラーの製造に使用する導電性ペーストとして、以下に示す方法により、金属微粒子と分散剤との複合体と、溶媒とを含むものを製造した。
酢酸銅(II)-水和物(3.00g、15.0mmol)(東京化成工業社製)、式(1)で示されるエチル3-(3-(メトキシ(ポリエトキシ)エトキシ)-2-ヒドロキシプロピルスルファニル)プロピオナート〔ポリエチレングリコールメチルグリシジルエーテル(ポリエチレングリコール鎖の分子量2000(炭素数91))への3-メルカプトプロピオン酸エチルの付加化合物〕(0.451g)、およびエチレングリコール(10mL)(関東化学社製)からなる混合物に、窒素を50mL/分の流量で吹き込みながら加熱し、125℃で2時間通気攪拌して脱気した。この混合物を室温に戻し、ヒドラジン水和物(1.50g、30.0mmol)(東京化成工業社製)を水7mLで希釈した希釈溶液を、シリンジポンプを用いて滴下した。希釈溶液は、約1/4量を2時間かけて滴下して一旦停止し、2時間攪拌して発泡が沈静化するのを確認した後、残量を更に1時間かけて滴下した。得られた褐色の溶液を60℃に昇温して、さらに2時間攪拌し、還元反応を終結させた。
上記の水分散液5mLをそれぞれ50mL三口フラスコに封入し、ウォーターバスを用いて40℃に加温しながら、減圧下で窒素を5mL/分の流速で流して、水を完全に除去し、銅微粒子複合体の乾燥粉末1.0gを得た。得られた銅微粒子複合体の乾燥粉末に、アルゴンガス置換したグローブバッグ内で30分間窒素バブリングしたエチレングリコール0.11gを、溶媒として添加した。銅微粒子複合体の乾燥粉末にエチレングリコールを添加した後、乳鉢で10分間混合し、金属微粒子含有率90%の導電性ペーストを得た。
合成した銅微粒子複合体の乾燥粉末2~25mgを、熱重量分析用アルミパンに精密にはかりとり、EXSTAR TG/DTA6300型示差熱重量分析装置(エスアイアイ・ナノテクノロジー株式会社製)に載せた。そして、不活性ガス雰囲気下において、室温~600℃まで毎分10℃の割合で昇温し、100℃~600℃の重量減少率を測定した。その結果から、銅微粒子複合体の乾燥粉末中に、3%のポリエチレンオキシド構造を含む有機物が存在することを確認した。
合成した銅微粒子複合体の平均一次粒子径を、TEM観察により測定した。まず、合成した銅微粒子複合体の乾燥粉末を、水で100倍に希釈して分散液とした。次に、分散液をカーボン膜被覆グリッド上にキャストして乾燥させ、透過型電子顕微鏡(装置:TEMJEM-1400(JEOL製)、加速電圧:120kV)にて観察した。そして、得られたTEM像の中から無作為に200個の銅微粒子複合体を抽出し、それぞれ面積を求め、真球に換算したときの粒子径を個数基準として算出し、平均一次粒子径とした。その結果、合成した銅微粒子複合体の平均一次粒子径は、42nmであった。
後述する実施例の導電性ピラーの製造方法を模擬して、上記の方法により得られた導電性ペーストの焼結体を作成した。具体的には、上記の方法により得られた導電性ペーストを、アルゴンガス雰囲気中でシリコンウエハ上に、膜厚が1mmとなるように均一に塗布した。
次に、シリコンウエハ上に塗布した導電性ペースト中の溶媒を低温で揮発させる仮焼成を行った。仮焼成は、窒素ガス雰囲気中で、卓上型真空はんだリフロー装置(ユニテンプ社製)を用いて、導電性ペーストの塗布されたシリコンウエハを120℃で5分間加熱することにより行った。
次に、シリコンウエハ上に塗布した導電性ペーストを焼結して、焼結体を形成した。導電性ペーストの焼結は、蟻酸蒸気を含む窒素雰囲気中で、卓上型真空はんだリフロー装置(ユニテンプ社製)を用いて、仮焼成後のシリコンウエハを250℃で10分間加熱することにより行った。
焼結体中の銅微粒子の平均粒子径の測定には、リガク社製のX線回折装置(商品名:SmartLab)を用いた。測定は、回折角度2θを0から4°までの範囲とし、ステップモードで行った。なお、ステップ角は0.005°、計測時間は5秒とした。
直径4インチのシリコンウエハ上に、スパッタ法によりTi(厚さ50nm)とCu(250nm)とがこの順に積層された電極パッドを形成し、電極パッドを有する基材とした。次に、電極パッドを有する基材の電極パッド側の面上に、レジスト樹脂を塗布してパターニングすることにより、直径30μmの円柱状の凹部からなる複数のレジスト開口部を有する膜厚30μmのレジスト層を形成した。レジスト開口部のアスペクト比(深さ:直径)は、1:1であった。
次に、柱状体を焼結して、上面に基材側に窪んだ凹型形状を有する焼結体を形成した。柱状体の焼結は、蟻酸蒸気を含む窒素雰囲気中で、卓上型真空はんだリフロー装置(ユニテンプ社製)を用いて、仮焼成後の基材を250℃で10分間加熱することにより行った。
以上の工程により、実施例の導電性ピラーを得た。
図6(A)において、符号11は基材、符号12は焼結体、符号12aは溝部、符号12bは上面、符号13は電極パッドを示す。図6(A)に示すように、実施例の導電性ピラー(焼結体12)は、上面12bが基材11側に窪んだ凹型形状であった。また、実施例の導電性ピラーの上面12bには、上面12bから基材11に向かって延出する複数の溝部12aが形成されていた。
また、図6(B)および図6(C)に示すように、実施例の導電性ピラーは、金属微粒子が焼結により融着した多孔質構造を有していた。
図7に示すように、実施例の導電性ピラー(焼結体12)の上面12bに形成された複数の溝部12a内に接合層となる材料22aが入り込み、溝部12a内に充填されてアンカー部が形成されていることが確認できた。また、焼結体12と接合層との界面に、金属間化合物層が形成されていることが確認できた。
図8に示すように、基材11と被接合部材21との間には、導電性ピラーの焼結体12と、焼結体12の凹部形状に沿って設けられた接合層22とを有する接合構造が形成されていた。
実施例の接合構造について以下に示す方法により「接合強度」「絶縁抵抗」「信頼性」を評価した。
「接合強度」
実施例の接合構造を8個(No.1~No.8)用意し、それぞれから接合試験片を採取した。そして、JIS Z-03918-5:2003「鉛フリーはんだ試験方法」に記載の方法で、各接合試験片にそれぞれせん断力を付加し、接合強度を測定した。その結果を表1に示す。
表1に示すように、実施例の接合構造は、いずれも接合強度が170~230MPaの範囲内であり、ばらつきが少なく、高い接合強度を有していることが確認できた。
実施例の接合構造について、温度130℃、相対湿度85%で3.7Vの電圧を96時間付与した時の絶縁抵抗を測定した。その結果、実施例の接合構造は、1MΩ以上の絶縁抵抗であって、抵抗変化率が10%未満であった。
このことから、実施例の接合構造は良好な抵抗値を示し、優れた信頼性を有していることが確認できた。
Claims (9)
- 基材上に設けられた金属微粒子の焼結体で構成され、
前記金属微粒子のX線小角散乱測定法を用いて測定した平均粒子径が1μm未満であり、
前記金属微粒子がチオエーテル型有機化合物を用いて分散されたものであり、
前記焼結体の上面から前記基材に向かって延出する複数の溝部を有し 、かつ、前記基材側に窪んだ凹型形状であることを特徴とする導電性ピラー。 - 前記金属微粒子が、AgおよびCuから選択される1種以上の金属であることを特徴とする請求項1に記載の導電性ピラー。
- 基材と、基材と対向配置される被接合部材との間に配置された接合構造であって、
基材上に設けられた金属微粒子の焼結体で構成され、金属微粒子のX線小角散乱測定法を用いて測定した平均粒子径が1μm未満であり、
前記金属微粒子がチオエーテル型有機化合物を用いて分散されたものであり、
焼結体の上面から前記基材に向かって延出する複数の溝部を有し、かつ、前記基材側に窪んだ凹型形状である導電性ピラーと、
前記導電性ピラーの前記凹部形状に沿って設けられた接合層と、
前記溝部内に前記接合層の一部が充填されたアンカー部と、
を有することを特徴とする接合構造。 - 前記接合層が、Sn、Pb、AgおよびCuから選択される1種以上の金属を含有する合金からなることを特徴とする請求項3に記載の接合構造。
- 前記導電性ピラーと前記接合層との間に、金属間化合物層を有することを特徴とする請求項3または4に記載の接合構造。
- 請求項3~5のいずれか一項に記載の接合構造を含むことを特徴とする電子機器。
- 前記接合構造を複数含み、複数の接合構造のうち、一部または全部が異なる形状である
請求項6に記載の電子機器。 - 基材上に、チオエーテル型有機化合物を用いて分散された平均一次粒子径1μm未満の金属微粒子を用いて柱状体を形成する工程と、
焼結体を形成する工程の前に、前記柱状体の少なくとも表面を酸素濃度200ppm以上の酸素含有雰囲気に暴露する工程と、
前記柱状体を焼結して、上面に前記基材側に窪んだ凹型形状を有する焼結体を形成する工程と、
を有することを特徴とする導電性ピラーの製造方法。 - 前記金属微粒子が、AgおよびCuから選択される1種以上の金属であることを特徴とする請求項8に記載の導電性ピラーの製造方法。
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