JP6606514B2 - 金属粒子及び導電性材料の粒子を用いた導電性接合材料並びに導電性接合構造 - Google Patents
金属粒子及び導電性材料の粒子を用いた導電性接合材料並びに導電性接合構造 Download PDFInfo
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- JP6606514B2 JP6606514B2 JP2016572065A JP2016572065A JP6606514B2 JP 6606514 B2 JP6606514 B2 JP 6606514B2 JP 2016572065 A JP2016572065 A JP 2016572065A JP 2016572065 A JP2016572065 A JP 2016572065A JP 6606514 B2 JP6606514 B2 JP 6606514B2
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Description
(1) 金属ナノ粒子、導電性材料のミクロン粒子、及び溶媒を含む接合材料であって、前記ミクロン粒子を構成する導電性材料の熱膨張係数が、前記ナノ粒子を構成する金属の線熱膨張係数よりも小さく、かつ、導電性材料のミクロン粒子の平均粒子径が0.5〜10μmであることを特徴とする導電性接合材料。
(2) 前記ナノ粒子を構成する金属とミクロン粒子を構成する導電性材料との線熱膨張係数差が5×10−6/K以上であることを特徴とする前記(1)に記載の導電性接合材料。
(3) 前記金属ナノ粒子が、Ag、Au、Cu、Niのいずれか1種であることを特徴とする前記(1)又は(2) に記載の金属接合材料。
(4) 前記導電性材料のミクロン粒子が、金属あるいは金属ホウ化物のいずれか1種あるいは2種以上であることを特徴とする前記(1)〜(3)のいずれかに記載の導電性接合材料。
(5) 前記導電性材料のミクロン粒子が、W、Mo、Cr、TiB2、ZrB2のいずれか1種又は2種以上であることを特徴とする前記(1)〜前記(4)に記載の導電性接合材料。
(6) 前記導電性接合材料中に含まれる金属ナノ粒子及び導電性材料のミクロン粒子の合計に対する10〜80体積%が前記導電性材料のミクロン粒子であることを特徴とする前記(1)〜(5)のいずれかに記載の導電性接合材料。
(7) 前記(1)〜(6)のいずれかに記載の導電性接合材料を、第1被接合体と第2被接合体との間に配し、450℃以下に加熱して、前記第1被接合体と前記第2被接合体とを接合することを特徴とする導電性接合材料による接合方法。
(8) 前記(1)〜(6)のいずれかに記載の導電性接合材料で第1被接合体と第2被接合体とを接合する導電性接合構造であって、前記接合方向断面における前記ミクロン粒子由来の導電性材料と前記金属ナノ粒子由来の金属の合計に対する2〜90質量%が前記導電性材料であることを特徴とする導電性接合構造。
(9) 前記金属と前記導電性材料との線熱膨張係数差が5×10−6/K以上であることを特徴とする前記(8)に記載の導電性接合構造。
(10) 前記金属が、Ag、Au、Cu、及びNiのいずれか1種であることを特徴とする前記(8)又は前記(9)に記載の導電性接合構造。
(11) 前記導電性材料が、W、Mo、Cr、TiB2、及びZrB2のいずれか1種又は2種以上であることを特徴とする前記(8)〜前記(11)に記載の導電性接合構造。
〔金属ナノ粒子の粒径の測定方法〕
粒子をエタノールや水等の溶媒中に高分散させたスラリーを観察試料台に塗布し、真空乾燥等の方法によって十分に乾かし、高分解能SEM(Scanning Electron Microscope)あるいはTEM(Transmission Electron Microscope)観察用サンプルを調製する。このようにして調製された観察用サンプルについて、粒子の直径×約10倍の視野範囲(例えば、視野角1270nm×950nmのSEM画像)で観察し、SEM画像あるいはTEM画像を取得する。取得した画像を紙に印刷し、画像中のスケールバーの長さとそれぞれの粒子の直径を定規で測定する。スケールバーより粒径を実際の大きさに換算し、算術平均により粒子の平均粒径を算出する。
第1被接合体1と第2被接合体2の熱膨張量に差が生じた場合、接合層3の熱膨張量を金属ナノ粒子及び導電性材料のミクロン粒子5の合計に対する前記導電性ミクロン粒子5の体積分の比率で調整することができ、第1被接合体1と第2被接合体2との間の熱膨張量の差を緩和することができ、これによってこれら第1被接合体1と第2被接合体2との間の接合強度の低下を未然に防止することができる。
また、接合層3の熱膨張量を第1被接合体1と第2被接合体2の熱膨張量の間の適切な値に調整できるので、金属ナノ粒子の金属焼結体からなる延性の低い接合層3の熱変形の程度であっても、第1被接合体1と第2被接合体2との間の熱膨張量の差を緩和することができ、第1接合層と第2接合層の初期接合強度の低下を防止することができる。
〔導電性ミクロン粒子の粒径の測定方法〕
導電性ミクロン粒子をエタノールや水等の溶媒中に高分散させたスラリーを観察試料台に塗布し、真空乾燥等の方法によって十分に乾かし、SEMあるいはTEM観察用サンプルを調製する。このようにして調製された観察用サンプルについて、粒子の直径×約10倍の視野範囲(例えば、視野角16.5μm×12.4μmのSEM画像)で観察し、SEM画像あるいはTEM画像を取得する。取得した画像を紙に印刷し、画像中のスケールバーの長さとそれぞれの粒子の直径を定規で測定する。スケールバーより粒径を実際の大きさに換算し、算術平均により粒子の平均粒径を算出する。
〔導電性接合材料中に含まれる金属ナノ粒子及び導電性材料のミクロン粒子の合計に対する導電性材料のミクロン粒子の体積%の測定方法〕
ナノ粒子を構成する金属の密度ρn、ミクロン粒子を構成する導電性材料の密度ρm、および、溶媒の密度ρyは既知である。ここで、ナノ粒子を被覆する有機殻は微量であるため無視する。導電性材料中に含まれるナノ粒子の合計質量Mn、ミクロン粒子の合計質量Mm、溶媒の質量Myとすると、ナノ粒子の体積Vn=質量Mn÷密度ρn、マイクロ粒子の体積Vm=質量Mm÷密度ρm、溶媒の体積Vy=質量My÷密度ρyで計算される。金属ナノ粒子及び導電性材料のミクロン粒子の合計体積はVn+Vmであり、この合計体積に対する導電性材料のミクロン粒子の割合はVm÷(Vn+Vm)で定義される。
また、接合層(接合構造)を構成する金属ナノ粒子及び導電性材料のミクロン粒子の合計体積分における導電性材料のミクロン粒子の体積割合は直接測定することができないため、代替として、接合方向の断面を出し、その断面における導電性材料と金属材料の合計に対する導電性材料の質量%を測定する。
〔接合方向断面における導電性材料と金属材料の合計に対する導電性材料の質量%の測定方法〕
先ず、導電性接合構造体を硬化性エポキシ樹脂等の樹脂中に埋め込み、樹脂を硬化させた後、第1被接合体から接合層を介して第2被接合体に至る積層方向に垂直に切断した試料片の切断面を研磨して、必要に応じてCP(Cross Section Polisher)加工を行い、切断面観察用のSEM観察試料片を作製する。
次に、作製された観察試料片をSEM観察試料台にセットし、その切断面を5000倍で観察し、その切断面画像を取得するとともに、SEM装置付随のEDX(Energy Dispersive X-ray Spectroscopy)により元素定量分析を行う。定量分析により得られる金属元素Aの質量%をMa、および、導電性材料の金属元素B(例えば、TiB2の場合、Tiを指す)の質量%をMb、導電性材料の金属以外の元素C(例えば、TiB2の場合、Bを指す)の質量%をMcとすると、導電性材料と金属材料の合計に対する導電性材料の質量%は、(Mb+Mc)/(Ma+Mb+Mc)で定義される。これらの動作を3〜10個の切断面において実施し、算術平均により前記質量%を求める。
表1に示す平均粒径の金属ナノ粒子と表1に示す平均粒径の導電性材料のミクロン粒子とを用い、また、溶媒としてテルペン系アルコールを用い、金属ナノ粒子と導電性材料のミクロン粒子とが表1に示す割合で配合されていると共に、これら金属ナノ粒子と導電性材料のミクロン粒子の合計割合が50体積%である導電性接合材料を調製した。なお、表1において、金属ナノ粒子及び導電性材料のミクロン粒子以外の成分は、上記の溶媒及び金属ナノ粒子を被覆する有機殻である。
接合を完了して作製された直後の各実施例及び比較例の導電性接合構造体について、常温まで冷却した後、ボンドテスター(デイジ社製シリーズ4000)を用い、ダイ・シェアモードにてSi半導体デバイスのせん断強度(n=10)を測定した。結果を表1に示す。本発明の各実施例においては、いずれも10MPa以上であった。これに対して、各比較例においては、せん断強度が10MPa以下と低い値であった。この結果、本発明の各実施例の導電性接合構造体においては、接合層の熱膨張係数が低減されており、接合後に良好なせん断強度が発現することが判明した。
上記接合を完了して作製された直後の各実施例及び比較例の導電性接合構造体について、気相式冷熱衝撃試験機(エスペック社製TSA-ES72-W)を使用し、−40℃と250℃で各々30分間ずつ保持する温度サイクル試験を行った。この温度サイクル試験の間、100サイクル経過ごとに導電性接合構造体を取り出し、超音波映像装置(日立パワーソリューションズ社製FineSAT)により、第1被接合体と接合層との間及び接合層と第2被接合体との間における剥離状態を調査し、1000サイクル後に剥離面積の増加率が初期状態を基準にして20%未満の場合を〇、また、この剥離面積の増加率が20%以上の場合を×として評価した。結果を表1に示す。
Claims (6)
- 金属ナノ粒子、導電性材料のミクロン粒子、及び溶媒を含む接合材料であって、前記ミクロン粒子を構成する導電性材料の線熱膨張係数が、前記ナノ粒子を構成する金属の線熱膨張係数よりも5×10−6/K以上小さく、かつ、導電性材料のミクロン粒子の平均粒子径が0.5〜10μmであり、前記導電性接合材料中に含まれる金属ナノ粒子及び導電性材料のミクロン粒子の合計に対する10〜80体積%が前記導電性材料のミクロン粒子であること、および
前記導電性材料のミクロン粒子が、W、Mo、Cr、TiB2、及びZrB2のいずれか1種又は2種以上であること、
を特徴とする導電性接合材料。 - 前記金属ナノ粒子が、Ag、Au、Cu、Niのいずれか1種であることを特徴とする請求項1に記載の導電性接合材料。
- 請求項1又は2に記載の導電性接合材料を、第1被接合体と第2被接合体との間に配し、450℃以下に加熱して、前記第1被接合体と前記第2被接合体とを接合することを特徴とする導電性接合材料による接合方法。
- 請求項1又は2に記載の導電性接合材料で第1被接合体と第2被接合体とを接合する導電性接合構造であって、前記接合方向断面における前記ミクロン粒子由来の導電性材料と前記金属ナノ粒子由来の金属の合計に対する2〜90質量%が前記導電性材料であることを特徴とする導電性接合構造。
- 前記金属と前記導電性材料との線熱膨張係数差が5×10−6/K以上であることを特徴とする請求項4に記載の導電性接合構造。
- 前記金属が、Ag、Au、Cu、及びNiのいずれか1種であることを特徴とする請求項4又は5に記載の導電性接合構造。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2015012399 | 2015-01-26 | ||
JP2015012399 | 2015-01-26 | ||
PCT/JP2016/052203 WO2016121764A1 (ja) | 2015-01-26 | 2016-01-26 | 金属粒子及び導電性材料の粒子を用いた導電性接合材料並びに導電性接合構造 |
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