JPWO2019093427A1 - 接合体の製造方法及び接合材 - Google Patents
接合体の製造方法及び接合材 Download PDFInfo
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Abstract
(M1−M2)/M1×100≧1.0 (I)
[式(I)中、M1は、第2の工程において、接合材の温度が焼結温度に到達した時の接合材の質量を示し、M2は、接合材中の不揮発分量を示す。]
Description
(M1−M2)/M1×100≧1.0 (I)
[式(I)中、M1は、第2の工程において、接合材の温度が焼結温度に到達した時の接合材の質量を示し、M2は、接合材中の不揮発分量を示す。]
(M1−M2)/M1×100≧1.0 (I)
本実施形態の接合材は、少なくとも金属粒子及び有機化合物を含有する。接合材は、例えば、金属ペースト(例えば銅ペースト)であり、無加圧接合用の金属ペースト(例えば銅ペースト)である。
金属粒子としては、サブマイクロ銅粒子、マイクロ銅粒子、これらの銅粒子以外のその他の金属粒子等が挙げられる。金属粒子は、優れた導電性及び接合性が得られる観点から、銅粒子(実質的に銅のみからなる粒子)を含むことが好ましく、サブマイクロ銅粒子及びマイクロ銅粒子を含むことがより好ましい。特に、サブマイクロ銅粒子とマイクロ銅粒子とを併用する場合、乾燥に伴う体積収縮及び焼結収縮が抑制されやすく、接合材の焼結時に接合材が接合面から剥離しにくくなる。すなわち、サブマイクロ銅粒子とマイクロ銅粒子とを併用することで、接合材を焼結させたときの体積収縮が抑制され、接合体はより充分な接合強度を有することができる。サブマイクロ銅粒子とマイクロ銅粒子とを併用した接合材をマイクロデバイスの接合に用いる場合は、マイクロデバイスがより良好なダイシェア強度及び接続信頼性を示す傾向がある。本明細書では、便宜上、複数の金属粒子の集合を「金属粒子」と称することがある。サブマイクロ銅粒子、マイクロ銅粒子及びその他の金属粒子についても同様である。
サブマイクロ銅粒子は、0.01μm以上1.00μm未満の粒径を有する銅粒子である。サブマイクロ銅粒子は、好ましくは、150℃以上300℃以下の温度範囲で焼結性を有する。サブマイクロ銅粒子は、粒径が0.01〜0.80μmの銅粒子を含むことが好ましい。サブマイクロ銅粒子は、粒径が0.01〜0.80μmの銅粒子を10質量%以上含んでいてよく、20質量%以上含んでいてもよく、30質量%以上含んでいてもよく、100質量%含んでいてもよい。銅粒子の粒径は、例えば、SEM像から算出することができる。銅粒子の粉末を、SEM用のカーボンテープ上にスパチュラで載せ、SEM用サンプルとする。このSEM用サンプルをSEM装置により5000倍で観察する。このSEM像の銅粒子に外接する四角形を画像処理ソフトにより作図し、その一辺をその粒子の粒径とする。
表面処理剤の処理量(質量%)=(W1−W2)/W1×100
マイクロ銅粒子は、1μm以上50μm未満の粒径を有する銅粒子である。マイクロ銅粒子は、粒径が2.0〜50μmの銅粒子を含むことが好ましい。マイクロ銅粒子は、粒径が2.0〜50μmの銅粒子を50質量%以上含んでいてよく、70質量%以上含んでいてもよく、80質量%以上含んでいてもよく、100質量%含んでいてもよい。
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としては、例えば、銅ナノ粒子、ニッケル、銀、金、パラジウム、白金等の粒子が挙げられる。その他の金属粒子の体積平均粒径は、0.01〜10μm、0.01〜5μm又は0.05〜3μmであってよい。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。その他の金属粒子の含有量は、充分な接合性を得る観点から、金属粒子の全質量を基準として、20質量%未満であってよく、10質量%以下であってもよく、0質量%であってもよい。
有機化合物は、例えば、接合材をペースト状とする機能、及び、第1の部材と第2の部材とが完全に接合されるまでの間、両部材をより安定的に仮止めする機能を有する。有機化合物は、第2の工程において接合材の温度が焼結温度に到達した時に、接合材の全質量を基準として1質量%以上残存する。例えば、有機化合物は、第2の工程において接合材の温度が焼結温度に到達した時に、接合材の全質量を基準として1質量%以上残存し得る有機化合物を含む。このような有機化合物としては、例えば、300℃以上の沸点を有する有機溶剤(以下、「第1の有機溶剤」ともいう。)及び還元雰囲気下での5%重量減少温度が100℃以上である熱分解性樹脂(以下、「第1の熱分解性樹脂」ともいう。)が挙げられる。本明細書中、有機溶剤とは、金属粒子の分散媒として機能する有機化合物を意味し、熱分解性樹脂とは、熱により分解する樹脂を意味する。
第1の有機溶剤の沸点は、300℃以上である。そのため、第1の有機溶剤は、焼結温度(例えば150〜300℃)まで接合材中に残存し、接合材に密着性及び可撓性を付与すると考えられる。第1の有機溶剤の沸点は、上記効果がより一層奏される観点から、好ましくは310℃以上である。第1の有機溶剤の沸点は、好ましくは450℃以下であり、より好ましくは400℃以下である。有機溶剤は、沸点以下の温度であってもその蒸気圧によって揮発して除去される。焼結温度が例えば150〜300℃である場合、上記沸点が450℃以下の溶剤は、焼結温度到達後には、充分な揮発速度で速やかに除去され、接合材中に残存し難い。その結果、接合材中に残存した有機溶剤によって焼結が阻害されることがなく、良好な接合状態で第1の部材と第2の部材とを接合することができる。これらの観点から、300℃以上の沸点を有する有機溶剤の沸点は、300〜450℃、300〜400℃、310〜450℃又は310〜400℃であってよい。
第1の熱分解性樹脂の還元雰囲気下(例えば、水素、ギ酸等を含む還元性ガス雰囲気下)での5%重量減少温度(以下、「5%重量減少温度」ともいう。)は100℃以上である。そのため、第1の熱分解性樹脂は、焼結温度(例えば150〜300℃)まで接合材中に一定量以上残存し、接合材に密着性及び可撓性を付与すると考えられる。第1の熱分解性樹脂の5%重量減少温度は、上記効果がより一層奏される観点及び式(I)の条件を満たすことが容易となる観点から、好ましくは150℃以上であり、より好ましくは200℃以上である。第1の熱分解性樹脂の5%重量減少温度は、式(I)の条件を満たすことが容易となる観点から、焼結温度より低いことが好ましい。具体的には、300℃以下が好ましく、250℃以下がより好ましい。これらの観点から、第1の熱分解性樹脂の5%重量減少温度は、100〜300℃、150〜300℃、200〜300℃、100〜250℃、150〜250℃又は200〜250℃であってよい。なお、熱分解性樹脂の還元雰囲気下での5%重量減少温度は、熱重量測定/示差熱分析(TG/DTA)装置を用いたTG/DTA測定によって測定することができる。
接合材は、添加剤として、金属粒子、表面処理剤、有機溶剤及び熱分解性樹脂以外のその他の成分(例えば、表面処理剤、有機溶剤及び熱分解性樹脂以外のその他の有機化合物)を更に含有していてもよい。添加剤としては、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;表面張力調整剤;アルキルアミン、アルキルカルボン酸等の分散剤;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が挙げられる。添加剤の含有量は、本発明の効果を阻害しない範囲で適宜調整することができる。
上述した接合材は、上述の金属粒子、有機化合物及び任意の成分(添加剤等)を混合して調製することができる。例えば、熱分解性樹脂及び有機溶剤を用いる場合、熱分解性樹脂を有機溶剤に溶解した後、得られた溶液に金属粒子(例えば、サブマイクロ銅粒子、マイクロ銅粒子、その他の金属粒子等)並びに任意の添加剤を添加し、分散処理を行うことで接合材を調製してよい。また、熱分解性樹脂を有機溶剤に溶解して得られた溶液と、金属粒子(例えば銅粒子)を有機溶剤に混合した後、分散処理を行うことで得られた分散液と、を混合することにより接合材を調製してもよい。この際、複数種の金属粒子を用いる場合には、複数の分散液を調製して混合してよく、熱分解性樹脂を含む溶液又は熱分解性樹脂を含む溶液と金属粒子を含む分散液との混合液に他の金属粒子を添加してもよい。また、任意の添加剤を用いる場合には、該添加剤は、熱分解性樹脂を含む溶液、金属粒子を含む分散液又は熱分解性樹脂を含む溶液と金属粒子を含む分散液との混合液に添加してよい。
次に、図面を参照して本実施形態の接合体の製造方法の各工程について説明する。図1は、一実施形態の接合体の製造方法を示す模式断面図である。図2及び図3は第1の工程の一例を示す模式断面図である。
第1の工程では、第1の部材10と、第2の部材20と、接合材(接合部)30と、を備える積層体50を用意する(図1(a)参照。)。
第2の工程では、積層体50を加熱して、所定の焼結温度で接合材30を焼結させて焼結体31とする。これにより、第1の部材10と、第2の部材20と、金属ピラー11及び電極パッド21の間に設けられた、焼結体(接合部)31と、を備える接合体100を得る(図1(b)参照。)。接合体100において、金属ピラー11と電極パッド21とは、焼結体31によって電気的に接続されている。
(接合材(無加圧接合用銅ペースト)の調製)
サブマイクロ銅粒子を含む材料としてCH−0200(50%体積平均粒径:0.36μm、三井金属社製)12.32g(61.6質量%)、イソボルニルシクロヘキサノール(沸点:308℃、日本テルペン化学株式会社製の「MTPH」、以下「MTPH」と略す)1.2g(6.0質量%)、及び、テルピネオール(沸点:214℃、和光純薬工業株式会社製)1.2g(6.0質量%)を、2000rpm、1分間の条件で株式会社シンキー製攪拌機(商品名:「あわとり練太郎 ARE−310」、以下同様。)にて混合した。その後、3本ロールミルで10回分散処理を行い、混合物を得た。
基板(WALTS−KIT CC80 Mark II−0201JY)及びはんだが付いていないチップ(WALTS−TEG CC80 Mark II−0101JY STD、Cuピラー径:φ25μm、Cuピラー高さ:25μm)の質量を計測後、基板の電極パッドに、厚さ50μmのステンレスマスクを用いて接合材をステンシル印刷した。次いで、接合材の印刷物上にチップをフリップチップボンダー(FCB3、パナソニック株式会社製)により搭載し、積層体を得た。積層体の質量を測定し、積層体の質量から基板及びチップの質量を引くことにより接合材の質量を求めた。
得られた積層体を、雰囲気制御可能なチューブオーブン(株式会社アールデック製)に設置し、水素雰囲気下で加熱処理した。加熱処理は、接合材の温度が焼結温度となるようにチューブオーブンの温度を設定し、接合材の温度を室温(25℃)から焼結温度(250℃)まで15分で昇温し、焼結温度(250℃)で60分間保持することにより行った。これにより、接合体を得た。
[接合材の焼結温度到達時の質量M1の測定]
第1の工程と同様にして作製した積層体を、雰囲気制御可能なチューブオーブン(株式会社アールデック製)に設置し、水素雰囲気下で加熱処理した。加熱処理は、接合材の温度が焼結温度となるようにチューブオーブンの温度を設定し、室温(25℃)から焼結温度(250℃)まで15分で昇温することにより行った。焼結温度に到達した時点で積層体を取り出し、真鍮ブロック上で急速冷却した。冷却後の積層体の質量を測定した。冷却後の積層体の質量から基板及びチップの質量を引くことにより、接合材の焼結温度到達時の質量M1を求めた。
磁性るつぼに接合材を入れ、磁性るつぼの風袋質量と接合材を入れた磁性るつぼの質量との差から、接合材の質量を得た。次いで、接合材を入れた磁性るつぼをチューブオーブン(株式会社アールデック製)に設置し、減圧水素置換後、水素中、300℃で2時間保持することにより接合材を処理した。チューブオーブン内を室温まで冷却し、減圧空気置換した後、接合材を入れた磁性るつぼを取り出した。処理後の磁性るつぼの質量と磁性るつぼの風袋質量との差から、処理後の接合材の質量(接合材中の不揮発分量)を得た。下記式より、接合材の不揮発分割合を求め、得られた不揮発分割合及び積層体の作製に用いた接合材の質量から、積層体に用いた接合材中の不揮発分量M2を算出した。
不揮発分割合(質量%)=([接合材中の不揮発分量]/[加熱前の接合材の質量])×100
[電気導通性評価]
接合体のディジーチェーン部分における両端の導通をマルチメータで確認した。導通を確認できた場合を良好(A)、導通を確認できなかった場合(断線している場合)を不良(B)と判定した。なお、上記評価では、印荷電圧5Vの条件で行い、抵抗値が100Ω以下である場合を導通有りと判定した。結果を表1に示す。
接合体をカップ内にサンプルクリップ(Samplklip I、ITW社製)で固定し、接合体の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)を接合体全体が埋まるまで流し込んだ。得られたサンプルを真空デシケータ内に静置し、1分間減圧することにより脱泡処理を行った。その後、室温下(25℃)10時間放置することによりエポキシ注形樹脂を硬化させた。これにより硬化サンプルを得た。
有機溶剤の割合(MTPH及びテルピネオールの添加量)を表1に示す量に変更したこと以外は、実施例1と同様にして接合材を調製した。得られた接合材を用いたこと以外は、実施例1と同様にして接合体を作製し、実施例1と同様に接合材の評価及び接合体の接合状態評価を行った。結果を表1に示す。
第1の工程(積層体の作製)後、第2の工程(接合材の焼結)の前に、表2に示す条件で乾燥工程を実施したこと以外は、実施例1と同様にして、接合体の作製、接合材の評価及び接合体の接合状態評価を行った。結果を表2に示す。
MTPHに代えてポリ(プロピレンカーボネート)(Sigma−Aldrich社製、5%重量減少温度:190℃)を用いたこと、テルピネオールに代えて炭酸プロピレン(和光純薬工業株式会社製、製品名「4−メチル−1、3−ジオキソラン−2−オン」)を用いたこと、2L3Nに代えてMA−025KFD(50%体積平均粒径:5μm、三井金属社製)を用いたこと、及び、各成分の含有量が表3に示す値となるように各成分を配合したこと以外は、実施例1と同様にして接合材を調製した。得られた接合材を用いたこと、第1の工程後、第2の工程の前に、表3に示す条件で乾燥工程を実施したこと、及び、第2の工程における焼結温度及び焼結時間を表3に示す条件に変更したこと以外は、実施例1と同様にして、接合体の作製、接合材の評価及び接合体の接合状態評価を行った。結果を表3に示す。
MTPHに代えてKFA−2000(アクリル系樹脂、5%重量減少温度:220℃、互応化学工業株式会社製)に変更したこと、及び、各成分の含有量が表4に示す値となるように各成分を配合したこと以外は、実施例1と同様にして接合材を調製した。得られた接合材を用いたこと、第1の工程後、第2の工程の前に、表4に示す条件で乾燥工程を実施したこと、及び、第2の工程における焼結温度及び焼結時間を表4に示す条件に変更したこと以外は、実施例1と同様にして、接合体の作製、接合材の評価及び接合体の接合状態評価を行った。結果を表4に示す。
有機溶剤のMTPHをトリブチリンに変更した又はMTPHを使用しなかったこと、及び、各成分の配合量を表5に示す量に変更したこと以外は、実施例1と同様にして接合材を調製した。得られた接合材を用いたこと以外は、実施例1と同様にして接合体を作製し、実施例1と同様に接合材の評価及び接合体の接合状態評価を行った。結果を表5に示す。
有機溶剤のMTPHをステアリン酸ブチルに変更したこと、及び、各成分の配合量を表5に示す量に変更したこと以外は、実施例1と同様にして接合材を調製した。得られた接合材を用いたこと以外は、実施例1と同様にして接合体を作製し、実施例1と同様に接合材の評価及び接合体の接合状態評価を行った。結果を表6に示す。
Claims (13)
- 表面に金属ピラーが設けられた第1の部材と、表面に電極パッドが設けられ、前記金属ピラーと前記電極パッドとが互いに対向するように配置された第2の部材と、前記金属ピラーと前記電極パッドとの間に設けられた、金属粒子及び有機化合物を含有する接合材と、を備える積層体を用意する第1の工程と、
前記積層体を加熱して、所定の焼結温度で前記接合材を焼結させる第2の工程と、を備え、
前記接合材は、下記式(I)の条件を満たす、接合体の製造方法。
(M1−M2)/M1×100≧1.0 (I)
[式(I)中、M1は、前記第2の工程において、前記接合材の温度が前記焼結温度に到達した時の前記接合材の質量を示し、M2は、接合材中の不揮発分量を示す。] - 前記有機化合物は、300℃以上の沸点を有する有機溶剤及び還元雰囲気下での5%重量減少温度が100℃以上である熱分解性樹脂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に記載の接合体の製造方法。
- 前記熱分解性樹脂は、ポリカーボネート、ポリ(メタ)アクリル酸、ポリ(メタ)アクリル酸エステル及びポリエステル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2に記載の接合体の製造方法。
- 前記有機溶剤の含有量及び前記熱分解性樹脂の含有量の合計は、前記接合材の全質量を基準として、1.0質量%以上である、請求項2又は3に記載の接合体の製造方法。
- 前記焼結温度は150〜300℃である、請求項1〜4のいずれか一項に記載の接合体の製造方法。
- 前記第2の工程では、無加圧又は0.1MPa以下の加圧下で前記接合材を焼結させる、請求項1〜5のいずれか一項に記載の接合体の製造方法。
- 前記金属粒子は、体積平均粒径が0.11〜0.80μmであるサブマイクロ銅粒子と、体積平均粒径が2.0〜50μmであり、アスペクト比が3.0以上であるフレーク状のマイクロ銅粒子と、を含み、
前記サブマイクロ銅粒子の含有量は、前記金属粒子の全質量を基準として、30〜90質量%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、10〜50質量%である、請求項1〜6のいずれか一項に記載の接合体の製造方法。 - 金属ピラーと電極パッドとを接合するために用いられる接合材であって、
前記接合材は、金属粒子と、300℃以上の沸点を有する有機溶剤及び還元雰囲気下での5%重量減少温度が100℃以上である熱分解性樹脂からなる群より選択される少なくとも一種を含む有機化合物と、を含有する、接合材。 - 前記熱分解性樹脂は、ポリカーボネート、ポリ(メタ)アクリル酸、ポリ(メタ)アクリル酸エステル及びポリエステル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8に記載の接合材。
- 前記有機溶剤の含有量及び前記熱分解性樹脂の含有量の合計は、前記接合材の全質量を基準として、1.0質量%以上である、請求項8又は9に記載の接合材。
- 前記金属粒子は、体積平均粒径が0.11〜0.80μmであるサブマイクロ銅粒子と、体積平均粒径が2.0〜50μmであり、アスペクト比が3.0以上であるフレーク状のマイクロ銅粒子と、を含み、
前記サブマイクロ銅粒子の含有量は、前記金属粒子の全質量を基準として、30〜90質量%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、10〜50質量%である、請求項8〜10のいずれか一項に記載の接合材。 - 150〜300℃の焼結温度で焼結させることで、前記金属ピラーと前記電極パッドとを接合するために用いられる、請求項8〜11のいずれか一項に記載の接合材。
- 無加圧又は0.1MPa以下の加圧下で焼結させることで、前記金属ピラーと前記電極パッドとを接合するために用いられる、請求項8〜12のいずれか一項に記載の接合材。
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