JP5651113B2 - 金属ナノ粒子を用いた接合材および接合方法 - Google Patents
金属ナノ粒子を用いた接合材および接合方法 Download PDFInfo
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- JP5651113B2 JP5651113B2 JP2011522632A JP2011522632A JP5651113B2 JP 5651113 B2 JP5651113 B2 JP 5651113B2 JP 2011522632 A JP2011522632 A JP 2011522632A JP 2011522632 A JP2011522632 A JP 2011522632A JP 5651113 B2 JP5651113 B2 JP 5651113B2
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- metal nanoparticles
- bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
- B23K35/24—Selection of soldering or welding materials proper
- B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
- B23K35/3006—Ag as the principal constituent
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- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
- B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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Description
本発明に用いる微小銀粒子含有組成物は、炭素数6〜8のカルボン酸、もしくはその誘導体と結合した銀ナノ粒子からなる。このような構成により、乾燥時や極性溶媒への分散時に当該組成物中の微小銀粒子が凝集せずに安定して存在することができる。
本工程では、液を二種用意する。一方は還元性を有する物質を溶解させた液I(後には還元液と称する)であり、もう一方は原料である金属塩(特に銀塩)が溶解された液II(後には原料液と称する)である。還元液は、上述の還元剤を純水に溶解させるとともに、保護剤および安定化剤のアンモニア水をそれぞれ添加し、均一になるまで混合することによって得る。また、原料液は金属塩の結晶を純水に溶解させることによって得られる。なお、保護剤の溶解性等に応じて、添加順を前後させても特段問題にはならない。
液をおのおの準備した後に、ウオーターバスもしくはヒーターを用いて液を昇温し、反応温度まで上昇させる。このとき、還元液と原料液は同様に加熱しておけば、温度差による対流によって一挙に混合できなくなるという問題を防止できる。また温度の違いによって生じる、反応の不均一が防止される効果もあり、粒子の均一性を保つことができるので好ましい。このときに昇温させる目的の温度(後の反応温度)は、40〜80℃の範囲である。
液がともに目的温度まで上昇すれば、還元液に対して原料液を添加する。添加は突沸に注意した上で、一挙に行うことが反応の均一性の面から好ましい。
反応液を混合した後、10〜30分程度攪拌を続け、粒子の成長を完結させる。このときの反応は、サンプリングした反応液に対し、ヒドラジンを滴下することにより、未還元銀の反応が生じるかどうか確認することによって、終点を判断する。
得られたスラリーは遠心分離機を用いて粒子を強制的に沈降させ固液分離を行なう。遠心分離は回転数3000rpmで30分間の処理をすることにより行なう。固液分離後上澄みを廃棄し、純水を加え、超音波分散機で10分間分散する。遠心分離、上澄み廃棄、純水添加、超音波分散という工程を3回行うことで、粒子に付着している余分な有機物質の除去を行う。
得られた金属塊(銀塊)を、60℃で12時間、大気中で乾燥することで、乾燥した金属粒子塊が得られる。
上述のような方法を用いて得られた金属粒子塊を、極性溶媒である、水、アルコール、ポリオール、グリコールエーテル、1−メチルピロリジノン、ピリジン、ターピネオール、ブチルカルビトール、ブチルカルビトールアセテート、テキサノール、フェノキシプロパノール、ジエチレングリコールモノブチルエーテル、ジエチレングリコールモノブチルエーテルアセテート等の分散媒へ添加することで分散液を作成する。
上記の工程を経て得られた接合材を接着面に塗布し、上下から加圧しつつ加温して、金属接着面の接合材を金属化する。加圧圧力は接合する物質が破壊されない限りにおいて高とするのがよい。
次に加圧した状態で、全体を150℃未満、より好ましくは100℃未満に加熱する。この加熱は接合材の溶媒を蒸発させる目的がある。従って、接着対象物全体を接合材に用いた溶媒の沸点より高い温度に加熱することが好ましい。加熱時間は加熱温度にもよるが、30秒〜30分でよい。
上記の工程を経て得られた接合材を接着面に塗布し、試験片をマウントした後、0.5Nで加圧した後、100℃で10分間乾燥した後に上下から10Nで加圧しつつ350℃で5分間加温して、金属接着面の接合材を金属化した。
接合の強度は、JISZ−03918−5:2003の「鉛フリーはんだ試験方法 第5部はんだ継ぎ手の引張およびせん断試験方法」に記載のある方法に準じて行った。すなわち、ダイボンディングされた被接合体を水平方向に押し、押される力に耐えかねて接合面が破断するときの力を算出する方法である。試験片は2mm□の銅チップを用いて行った。本参考例および実施例ではDAGE社製ボンドテスタを使用して試験を行っている。シェア高さは200μm、試験速度は5mm/min、測定は室温で行っている。
洗浄後のナノ粒子2質量部をシクロヘキサン96質量部とオレイン酸2質量部との混合溶液に添加し、超音波によって分散させた。分散溶液を支持膜付きCuマイクログリッドに滴下し、乾燥させることでTEM試料とした。作成したマイクログリッドを透過型電子顕微鏡(日本電子株式会社製:JEM−100CXMark−II型)を使用し、100kVの加速電圧で、明視野で粒子を観察した像を、倍率300,000倍で撮影した。
本参考例および実施例に共通して利用する銀ナノ粒子を次のようにして作製した。反応槽に5L反応槽を使用した。また、攪拌のために羽根のついた攪拌棒を反応槽中心に設置した。反応槽には温度をモニターするための温度計を設置し、また溶液に下部より窒素を供給できるようにノズルを配設した。
得られたヘキサン酸被覆銀粒子粉末(平均粒子径:13.9nm、X線結晶子径(株式会社Rigaku製X線回折装置:RINT−2100、Co管球によりCo−Kαの特性X線により観察し、Ag(111)面の回折線からシェラーの式を利用して算出:9.6nm)80gを、テルピネオール(構造異性体混合/和光純薬工業株式会社製)15g、湿潤分散剤としてDisperBYK(登録商標)−2020(ビックケミー・ジャパン株式会社製)5gを混合し、接合材を作成した。得られた接合材を印刷法によりガラス基板上に塗布した。このときの条件はメタルマスク(マスク厚50μmt)とし、メタルスキージは手動にて実施した。
ヘキサン酸覆銀粒子粉末、テルピネオール、分散剤量を質量割合で90:8.6:1.4にした他は参考例1と同様として接合材を作成した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。
ヘキサン酸覆銀粒子粉末、テルピネオール、分散剤量を質量割合で80:18.6:1.4にした他は参考例1と同様として接合材を作成した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。
ヘキサン酸被覆銀粒子粉末に変えて、ソルビン酸被覆銀粒子粉末(平均粒子径:35.7nm、X線結晶子径/Ag(111):30.2nm)(なお、当該粒子のTGチャートを図4に示す。これより当該粒子の焼結点は194℃であるとした。)を使用した。ソルビン酸覆銀粒子粉末、テルピネオール、分散剤量を質量割合で90:8.6:1.4にした他は参考例1と同様として接合材を作成した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。なお、当該接合材は光沢があり、展性に優れた接合材であることが確認された。
ソルビン酸覆銀粒子粉末、テルピネオール、分散剤量を質量割合で90:9.3:0.7にした他は参考例1と同様として接合材を作成した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。
ヘキサン酸被覆銀粒子粉末、ソルビン酸被覆銀粒子粉末、テルピネオール、分散剤量を45:45:8.6:1.4とした銀ナノ粒子接合材を作成し、参考例1と同様として接合材を作成した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。
金属ナノ粒子粉末に変えて、平均粒子径0.60μmの球状銀粉(銀マイクロ粒子)を用い、球状銀粉、テルピネオール、分散剤を90:8.6:1.4の比率とした接合材を作製した。その後、参考例1と同様の条件にて接合強度を測定した。得られた結果を表1にあわせて示す。
接合対象物の接合を市販の高温鉛はんだペースト(日本スペリア株式会社製のSN515RMA A M Q M−293T)で行った。接合方法は、参考例および実施例の場合と同様である。予備加熱は150℃で2分間行い、焼成工程での温度は350℃で40秒間行った。得られた結果を表1にあわせて示す。
接合対象物の接合を市販の鉛フリーはんだペースト(千住金属工業株式会社製のM705−K2−V)で行った。接合方法は、参考例および実施例の場合と同様である。予備加熱は150℃で2分間行い、焼成工程での温度は250℃で40秒間行った。得られた結果を表1にあわせて示す。
Claims (6)
- 平均粒径100nm以下で表面に炭素数6〜8の直鎖脂肪酸が被覆した金属ナノ粒子と、
前記金属ナノ粒子による粉末に対して5〜20質量%の極性溶媒とからなり、
前記金属ナノ粒子は異なる直鎖脂肪酸で被覆された少なくとも2種類以上の金属ナノ粒子が混合されたものであり、前記直鎖脂肪酸の1つは不飽和脂肪酸である接合材。 - さらに分散剤が添加される、請求項1に記載された接合材。
- 平均粒径100nm以下であり、表面に炭素数が6〜8の直鎖脂肪酸が被覆された金属ナノ粒子を極性溶媒中に分散した接合材を接着面もしくは被接着面、あるいはその双方に塗布する工程と、
接着対象物を前記接着面に圧接しながら、金属ナノ粒子の焼結温度以下に加熱する第1の加熱工程と、
加熱温度を200℃以上350℃以下に加熱する第2の加熱工程を有し、
前記金属ナノ粒子は異なる直鎖脂肪酸で被覆された少なくとも2種類異常の金属ナノ粒子が混合されたものであり、前記直鎖脂肪酸の1つは不飽和脂肪酸である接合方法。 - 平均粒径100nm以下であり、表面に炭素数が6〜8の直鎖脂肪酸が被覆された金属ナノ粒子を極性溶媒中に分散した接合材を接着面および被接着面に塗布する工程と、
前記接合面と被接合面を前記金属ナノ粒子の焼結温度以下で乾燥する第1の加熱工程と、
前記接合面および被接合面を突き合わせ、加圧しながら200℃以上350℃以下に加熱する第2の加熱工程を有し、
前記金属ナノ粒子は異なる直鎖脂肪酸で被覆された少なくとも2種類異常の金属ナノ粒子が混合されたものであり、前記直鎖脂肪酸の1つは不飽和脂肪酸である接合方法。 - 前記第1の加熱工程の保持時間が30秒以上30分以下であり、
前記第2の加熱工程の保持時間が30秒以上60分以下である請求項3または4に記載された接合方法。 - 前記金属ナノ粒子は銀ナノ粒子である請求項3〜5の何れかに記載された接合方法。
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KR20120039698A (ko) | 2012-04-25 |
US20120103515A1 (en) | 2012-05-03 |
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US8858700B2 (en) | 2014-10-14 |
CN102470490A (zh) | 2012-05-23 |
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