JP2021063274A - 接合材、接合材の製造方法及び接合体 - Google Patents
接合材、接合材の製造方法及び接合体 Download PDFInfo
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- JP2021063274A JP2021063274A JP2019188913A JP2019188913A JP2021063274A JP 2021063274 A JP2021063274 A JP 2021063274A JP 2019188913 A JP2019188913 A JP 2019188913A JP 2019188913 A JP2019188913 A JP 2019188913A JP 2021063274 A JP2021063274 A JP 2021063274A
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- Prior art keywords
- silver
- bonding material
- sintered body
- mass
- particle group
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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- H01L2224/32151—Disposition the layer connector connecting between a semiconductor or solid-state body and an item not being a semiconductor or solid-state body, e.g. chip-to-substrate, chip-to-passive
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Abstract
Description
そこで、本発明は、従来よりも優れた接合強度を有する接合体を作製することができる接合材、その接合材の製造方法、その接合材を用いた接合体を提供することを目的とする。
すなわち、本発明の第1の態様は、銀粉末が焼き固められた焼結体を含み、前記焼結体の気孔率が8〜30%であることを特徴とする、接合材である。
図1に示す接合体10は、導電体12と基板14とが接合材13により接合された積層体である。
本実施形態の接合体10は、接合材13に特徴があり、その他の構成については公知の種々の接合体を適宜適用できる。
本実施形態の接合材は、銀粉末が焼き固められた焼結体を含み、前記焼結体の気孔率が8〜30%である。
本明細書において、接合材とは、二つの物体を貼り合わせるものを包含し、典型的には導電体と基板との間に介在してこれらを貼り合わせるものが挙げられる。
焼結体の気孔率が上記範囲内であると、例えば導電体と基板との接合強度(接合体のシェア強度)を優れたものとすることができる。
ここで、シェア強度はJIS Z 3198−7:2003に準拠した方法により測定されたものを意味する。具体的な測定方法は実施例において後述する。
まず、焼結体を水に沈めて焼結体の体積を測定し、また、焼結体の質量を測定する。また、その質量に相当する焼結体が気孔を有しない場合の体積を、理論上の密度に基づいて算出する。測定した体積と、気孔を有しない場合の理論上の体積とから、焼結体の気孔率を算出する。
また、本実施形態の接合材は、接合を容易とするために、1mm以下の肉厚部分を有するものでもよい。
接合材の大きさは、特に限定されず、基板及び導電体の仕様に応じて適宜調整すればよい。接合材の形状が円板状である場合、円板の直径は、0.5〜50mmであることが好ましく、2〜30mmであることがより好ましい。接合材の形状が矩形板状である場合、長辺の長さは、0.5〜50mmであることが好ましく、2〜30mmであることがより好ましい。
実施例において後述するように、接合面の表面粗さRaが、上記範囲内であると、接合体のシェア強度を優れたものとすることができる。
接合材の接合面の表面粗さは、次のように測定することができる。超深度カラー3D形状測定顕微鏡(キーエンス、VK−9510)を用いて、接合材表面の任意の5箇所について、表面粗さを測定し、平均値を算出する。
加えて、係る焼結体は銀粉末の融点より高い温度下でも溶融しない。また、この焼結体を含む接合材を用いることにより、バルクの融点よりも低い温度で接合することができる。
本実施形態の接合材の製造方法は、溶剤と銀粉末との分散液を用いて形成した塗工膜を加熱して焼結体を得る工程を有する。
本実施形態の分散液は、溶剤に銀粉末が分散しているものである。
ここでの溶剤としては、例えば、水、アルコール系溶剤、グリコールエーテル系溶剤、テルピネオール類等が挙げられる。
アルコール系溶剤としてはイソプロピルアルコール、1,2−ブタンジオール、イソボルニルシクロヘキサノール、2,4−ジエチル−1,5−ペンタンジオール、2,2−ジメチル−1,3−プロパンジオール、2,5−ジメチル−2,5−ヘキサンジオール、2,5−ジメチル−3−ヘキシン−2,5−ジオール、2,3−ジメチル−2,3−ブタンジオール、1,1,1−トリス(ヒドロキシメチル)エタン、2−エチル−2−ヒドロキシメチル−1,3−プロパンジオール、2,2′−オキシビス(メチレン)ビス(2−エチル−1,3−プロパンジオール)、2,2−ビス(ヒドロキシメチル)−1,3−プロパンジオール、1,2,6−トリヒドロキシヘキサン、ビス[2,2,2−トリス(ヒドロキシメチル)エチル]エーテル、1−エチニル−1−シクロヘキサノール、1,4−シクロヘキサンジオール、1,4−シクロヘキサンジメタノール、エリトリトール、トレイトール、グアヤコールグリセロールエーテル、3,6−ジメチル−4−オクチン−3,6−ジオール、2,4,7,9−テトラメチル−5−デシン−4,7−ジオール等が挙げられる。
グリコールエーテル系溶剤としては、ジエチレングリコールモノ−2−エチルヘキシルエーテル、エチレングリコールモノフェニルエーテル、2−メチルペンタン−2,4−ジオール、ジエチレングリコールモノヘキシルエーテル、ジエチレングリコールジブチルエーテル、トリエチレングリコールモノブチルエーテル等が挙げられる。
ここでの銀粉末には、平均粒子径が相違する銀粒子群を組み合わせて用いることが好ましい。平均粒子径が相違するものを併用することで、特定の気孔率(8〜30%)を有する接合材を容易に作製できる。
銀粒子群の平均粒子径は、メディアン径D50の値を採用する。本発明において、各銀粉末のメディアン径D50は、SALD−2300(島津製作所製)を用いて、レーザー回折法により測定したもの(体積平均粒子径)を意味する。
例えば、平均粒子径が相違する第1の銀粒子群と第2の銀粒子群とを含み、第1の銀粒子群の平均粒子径が50nm以上1000nm未満であり、第2の銀粒子群の平均粒子径が1μm以上20μm未満であることが好ましい。
第2の銀粒子群の平均粒子径は、1μm以上20μm未満であり、好ましくは3μm以上15μm以下であり、より好ましくは3μm以上10μm以下である。
係る第1の銀粒子群と第2の銀粒子群との併用により、特定の気孔率(8〜30%)を有する接合材を容易に作製でき、接合強度の高められた接合体が得られやすくなる。
第3の銀粒子群の平均粒子径は、20μm以上60μm未満であり、好ましくは30μm以上50μm以下であり、より好ましくは35μm以上45μm以下である。
第1の銀粒子群及び第2の銀粒子群に加えて第3の銀粒子群をさらに併用することで、特定の気孔率(8〜30%)を有する接合材をより安定に作製できる。
本実施形態の銀粉末においては、第2の銀粒子群として、平均粒子径の異なる2種以上を用いることが好ましい。例えば、第2の銀粒子群として、平均粒子径が1μm以上10μm未満の銀粒子群と、平均粒子径が10μm以上20μm未満の銀粒子群と、を組み合わせて用いることが好ましい。
第2の銀粒子群の割合は、銀粉末の合計の質量(100質量%)に対して、30〜99質量%であることが好ましく、45〜90質量%がより好ましく、50〜90質量%がさらに好ましい。
第3の銀粒子群をさらに併用する場合、第3の銀粒子群の割合は、銀粉末の合計の質量(100質量%)に対して、1〜70質量%であることが好ましく、1〜50質量%がより好ましく、1〜45質量%がさらに好ましい。ただし、第1の銀粒子群、第2の銀粒子群及び第3の銀粒子群の割合の和は、100質量%を超えない。
本実施形態における、前記溶剤と前記銀粉末との分散液は、当該分散液中の前記溶剤の含有量が、5質量%以上25質量%以下であることが好ましく、より好ましくは5質量%以上20質量%以下であり、さらに好ましくは5質量%以上15質量%以下であり、特に好ましくは6質量%以上10質量%以下である。
分散液中の溶剤の含有量を5質量%以上25質量%以下とすることにより、気孔率が8〜30%の焼結体を容易に得ることができる。
分散液を焼結する際に、分散液中の溶剤は揮発して、焼結体中に気孔が形成される。分散液中の溶剤の含有量を上記範囲内とすることにより、焼結体の気孔率を8〜30%とすることができる。
本実施形態における、焼結体を得る工程では、溶剤と銀粉末との分散液を用いて形成した塗工膜を加熱して焼結体を得る。
基台の材料としては、例えば、ガラス、石英、シリコン、金属等が挙げられるが、これに限定されない。実施例において後述するように、金属としては、例えば、黄銅を用いることができるが、これに限定されない。
金属の基台を用いる場合、予め基台に潤滑離型剤を塗布しておくと、焼結体を基台から容易に剥がすことができる。
例えば、得られた焼結体表面の粗さを制御するため、焼結体を得る工程の後段側に、焼結体の表面を研磨する工程、又は、焼結体の表面に銀、銅、錫、金及びニッケルからなる群より選択される1種以上のめっきを施す工程をさらに有していてもよい。
焼結体の表面を研磨する方法としては、特に限定されず、例えば、化学研磨、電解研磨、機械研磨等が挙げられる。実施例において後述するように、2000番の研磨紙を用いて、焼結体の表面を研磨することにより、十分な接合強度を有する接合体を作製することができる接合材を得ることができる。
焼結体の表面にめっきを施す方法としては、特に限定されず、例えば、電気めっき、無電解めっき、真空めっき等が挙げられる。めっきの種類としては特に限定されないが、銀、銅、錫、金及びニッケルからなる群より選択される1種の金属又は、2種以上からなる合金をめっきすることが挙げられる。めっきを施す工程は、組成が異なる2層以上のめっきを重ねてめっきすることであってもよい。
実施形態(i)によれば、分散液中の前記溶剤の含有量を特定の割合とすることで、気孔率8〜30%の焼結体を含む接合材を容易に製造できる。
前記銀粉末は、例えば、第1の銀粒子群の割合が1〜50質量%であり、第2の銀粒子群の割合が50〜99質量%であってもよい。
前記銀粉末は、例えば、第1の銀粒子群の割合が5〜30質量%であり、第2の銀粒子群の割合が70〜95質量%であってもよい。
前記銀粉末は、例えば、第1の銀粒子群の割合が5〜15質量%であり、第2の銀粒子群の割合が85〜95質量%であってもよい。
前記第1の銀粒子群及び第2の銀粒子群の割合は、前記銀粉末の合計の質量(100質量%)に対する割合である。また、前記第1の銀粒子群及び第2の銀粒子群の割合の和は、100質量%を超えない。
実施形態(ii)によれば、特定の平均粒子径をもつ銀粒子群を組み合わせて用いることで、気孔率8〜30%の焼結体を含む接合材を容易に製造できる。
上述した銀粉末は、例えば、第1の銀粒子群の割合が1〜50質量%であり、第2の銀粒子群の割合が30〜98質量%であり、第3の銀粒子群の割合が1〜69質量%であってもよい。
上述した銀粉末は、例えば、第1の銀粒子群の割合が1〜30質量%であり、第2の銀粒子群の割合が30〜90質量%であり、第3の銀粒子群の割合が5〜60質量%であってもよい。
上述した銀粉末は、例えば、第1の銀粒子群の割合が3〜8質量%であり、第2の銀粒子群の割合が45〜72質量%であり、第3の銀粒子群の割合が20〜50質量%であってもよい。
上述した第1の銀粒子群、第2の銀粒子群及び第3の銀粒子群の割合は、銀粉末の合計の質量(100質量%)に対する割合である。また、第1の銀粒子群、第2の銀粒子群及び第3の銀粒子群の割合の和は、100質量%を超えない。
実施形態(iii)によれば、特定の平均粒子径をもつ銀粒子群を組み合わせて用いることで、気孔率8〜30%の焼結体を含む接合材を容易に製造できる。
本実施形態の接合体は、図1に示したように、導電体と、基板とが、上述した接合材により接合されているものである。
基板としては、回路基板、ガラス繊維強化エポキシ系プリント基板やポリイミド系の基板、セラミックス基板、メタル基板、Cuリードフレーム等が挙げられる。
接合する時の圧力としては、特に限定されないが、例えば、0.1MPa以上3MPa以下であってもよい。
接合時の雰囲気は、大気中で行われてもよく、窒素中で行われてもよい。
銀粉末として、以下に示す銀粒子群を用いた。
銀粒子群1A:平均粒子径 300nm
銀粒子群2A:平均粒子径 4μm
銀粒子群2B:平均粒子径 10μm
銀粒子群3:平均粒子径 42μm
銀粒子群1B:平均粒子径 50nm
銀粒子群1A、1B、2A、3の銀粒子の形状は球状であり、銀粒子群2Bの銀粒子の形状はフレーク状であった。
溶剤として、エチレングリコールを用いた。
上述した銀粒子群と溶剤とを、表1に示す組成で混合して、分散液1〜9を調製した。表1中、銀粒子群のそれぞれの値は、銀粉末の合計の質量に対する、各銀粒子群の質量の割合(質量%)を示す。また、溶剤の割合は、銀粉末と溶剤との合計の質量に対する、溶剤の質量の割合(質量%)を示す。
(実施例1)
分散液1を用いて、黄銅の基台上に塗工膜を作製した。
黄銅としては、65質量%の銅と、35質量%の亜鉛とからなるものを用いた。
焼結体を得る工程:
作製した塗工膜を、200℃で30分間、無加圧で加熱して焼結体を得た。ハサミを用いて、得られた焼結体を、小片(縦×横の寸法:3mm×3mm)に切断した。
研磨する工程:
得られた小片を、2000番の研磨紙(三共理化学製 耐水研磨紙シート)を用いて焼結体の表面を研磨し、接合材を得た。
焼結条件を250℃で30分間に変更した以外は、実施例1と同様にして接合材を得た。
分散液1を用いて、上述した黄銅の基台上に塗工膜を作製した。
焼結体を得る工程:
作製した塗工膜を、200℃で30分間、無加圧で加熱して焼結体を得た。
銀めっきを施す工程:
得られた焼結体を、2−エチルヘキシルアミンにアセト酢酸銀を溶解させた溶液に浸漬し、40℃で10分間、静置した。続いて、焼結体を混合液から取り出して乾燥させた。
焼結条件を250℃で30分間に変更した以外は、実施例3と同様にして接合材を得た。
用いる分散液を分散液2に変更した以外は、実施例1と同様にして接合材を得た。
焼結条件を250℃で30分間に変更した以外は、実施例5と同様にして接合材を得た。
用いる分散液を分散液2に変更した以外は、実施例3と同様にして接合材を得た。
焼結条件を250℃で30分間に変更した以外は、実施例7と同様にして接合材を得た。
用いる分散液を分散液3に変更した以外は、実施例2と同様にして接合材を得た。
用いる分散液を分散液4に変更した以外は、実施例2と同様にして接合材を得た。
焼結条件を250℃で90分間に変更した以外は、実施例5と同様にして接合材を得た。
用いる分散液を分散液5に変更した以外は、実施例2と同様にして接合材を得た。
用いる分散液を分散液6に変更した以外は、実施例2と同様にして接合材を得た。
分散液2を用いて、上述した黄銅の基台上に塗工膜を作製した。
焼結体を得る工程:
作製した塗工膜を、250℃で30分間、無加圧で加熱して焼結体を得た。
銅めっきを施す工程:
得られた焼結体を、窒素雰囲気中、2−エチルヘキシルアミンにギ酸銅(II)四水和物(和光純薬工業株式会社製、型番:LKJ3210、一次平均粒子径:20μm)を溶解させた溶液に浸漬し、140℃で10分間、静置した。続いて、焼結体を混合液から取り出して乾燥させた。
用いる分散液を分散液7に変更した以外は、実施例1と同様にして接合材を得た。
焼結条件を250℃で30分間に変更し、焼結時に0.4MPaで加圧しつつ焼結したた以外は、比較例1と同様にして接合材を得た。
焼結時に0.4MPaで加圧しつつ焼結した以外は、比較例1と同様にして接合材を得た。
焼結条件を250℃で30分間に変更した以外は、比較例1と同様にして接合材を得た。
用いる分散液を分散液7に変更し、焼結体の表面を研磨しなかった以外は、実施例1と同様にして接合材を得た。
焼結条件を250℃で30分間に変更した以外は、比較例5と同様にして接合材を得た。
用いる分散液を分散液8に変更し、焼結体の表面を研磨しなかった以外は、実施例2と同様にして接合材を得た。
用いる分散液を分散液8に変更した以外は、実施例2と同様にして接合材を得た。
用いる分散液を分散液9に変更し、焼結体の表面を研磨しなかった以外は、実施例2と同様にして接合材を得た。
用いる分散液を分散液9に変更した以外は、実施例2と同様にして接合材を得た。
接合材を水に沈めて接合材の体積を測定し、接合材の質量を測定した。また、その質量に相当する接合材が気孔を有しない場合の体積を、理論上の密度に基づいて算出した。測定した体積と、気孔を有しない場合の理論上の体積とから、気孔率を算出した。
超深度カラー3D形状測定顕微鏡(キーエンス、VK−9510)を用いて、接合材表面の任意の5箇所について、表面粗さを測定し、平均値を算出した。測定箇所の大きさは、1400μm×1050μmであった。
(実施例21〜34、比較例11〜20)
導電体として、Siチップ側から順に、Ti層(厚み40nm)及びAg層(厚み1000nm)がスパッタリングにより積層されたSiチップ(縦×横の寸法:3mm×3mm)を用いた。接合材として、実施例1〜14、比較例1〜10の各接合材を用いた。各接合材の厚さは100μmであった。基板として、銅基板を用いた。
基板、接合材、導電体を、接合材の研磨した面が接合面になるように、この順で重ねた後、大気中にて圧力を0.4MPaに設定し、温度250℃で加熱処理を施すことにより接合して、接合体を得た。実施例1〜14、比較例1〜10の各接合材を用いて、実施例21〜34、比較例11〜20の接合体を得た。
得られた実施例21〜34、比較例11〜20の接合体のシェア強度を、次に示す測定方法によって測定した。結果を表3に示す。
実施例21〜34、比較例11〜20の各接合体のシェア強度(せん断強度)を次のように測定した。測定結果を表3に示す。
シェア強度試験:
得られた各接合体について、万能型ボンドテスター NordsonDAGE Series4000(Nordson Corporation製)を使用して、室温(25℃)条件下、JIS Z 3198−7:2003に準拠した方法で、Siチップと基板との間のせん断強度(MPa)の測定を行った。各試料について5回測定を行い、せん断強度(MPa)の平均値を算出した。
導電体と、銀めっきした銅板とを、実施例1の接合材を用いて、大気中にて、圧力を0.4MPa又は1MPaに設定し、温度200℃、250℃、300℃でそれぞれ加熱処理を施すことにより接合して、接合体を得た。
導電体と、めっきが施されていない銅板(無垢銅板)とを、実施例14の接合材を用いて、窒素中にて、圧力を0.4MPa又は1MPaに設定し、温度250℃、300℃、350℃でそれぞれ加熱処理を施すことにより接合して、接合体を得た。
本発明の接合材は、従来の接合材では困難であった高温下(例えば300℃以上)での使用が可能であり、炭化ケイ素(SiC)を用いたパワー半導体などを備えた電子部品用の接合材として有用である。
Claims (8)
- 銀粉末が焼き固められた焼結体を含み、前記焼結体の気孔率が8〜30%である、接合材。
- 接合面の表面粗さRaが、500nm以上3.3μm以下である、請求項1に記載の接合材。
- 溶剤と銀粉末との分散液を用いて形成した塗工膜を加熱して焼結体を得る工程を有し、
前記分散液中の前記溶剤の含有量が、5質量%以上25質量%以下である、接合材の製造方法。 - 溶剤と銀粉末との分散液を用いて形成した塗工膜を加熱して焼結体を得る工程を有し、
前記銀粉末は、平均粒子径が相違する第1の銀粒子群と第2の銀粒子群とを含み、
前記第1の銀粒子群の平均粒子径が50nm以上1000nm未満であり、
前記第2の銀粒子群の平均粒子径が1μm以上20μm未満である、接合材の製造方法。 - 前記銀粉末は、さらに、平均粒子径が20μm以上60μm未満である第3の銀粒子群を含む、請求項4に記載の接合材の製造方法。
- 前記焼結体を得る工程において、前記塗工膜に加えられる圧力を5MPa以下としつつ、前記塗工膜を加熱する、請求項3〜5のいずれか一項に記載の接合材の製造方法。
- さらに、前記焼結体の表面を研磨する工程、又は、前記焼結体の表面に銀、銅、錫、金及びニッケルからなる群より選択される1種以上のめっきを施す工程を有する、請求項3〜6のいずれか一項に記載の接合材の製造方法。
- 導電体と、基板とが、請求項1又は2に記載の接合材により接合されている、接合体。
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