JP5957630B2 - 金属インク - Google Patents
金属インク Download PDFInfo
- Publication number
- JP5957630B2 JP5957630B2 JP2012503530A JP2012503530A JP5957630B2 JP 5957630 B2 JP5957630 B2 JP 5957630B2 JP 2012503530 A JP2012503530 A JP 2012503530A JP 2012503530 A JP2012503530 A JP 2012503530A JP 5957630 B2 JP5957630 B2 JP 5957630B2
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- JP
- Japan
- Prior art keywords
- ink
- copper
- nanoparticles
- metal
- substrate
- 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.)
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- 238000012360 testing method Methods 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010891 toxic waste Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 150000004072 triols Chemical group 0.000 description 1
- 231100000925 very toxic Toxicity 0.000 description 1
- 239000003039 volatile agent Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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Description
ルイス酸 + ルイス塩基 → ルイス酸/ルイス塩基錯体
小さいイオン半径の原子中心を有し、
高い正電荷を有し、
この種はそれらの原子価殻中に電子対を含有せず、
低い電子親和力を有し、
強く溶媒和される傾向があり、
高いエネルギーのLUMOを有する。
大きい半径を有し、
低いまたは不完全な正電荷を有し、
それらの原子価殻中に電子対を含有し、
分極および酸化し易く、
低いエネルギーのLUMOであるが大きな規模のLUMO係数を有する。
小さいが高度に溶媒和された3.0〜4.0の電気陰性の原子中心を有し、
弱く分極することができる種であり、
酸化し難く、
高いエネルギーのHOMOを有する。
2.5〜3.0の範囲の中程度の電気陰性度の大型の原子を有し、
分極および酸化し易く、
低いエネルギーのHOMOであるが、大きな規模のHOMO係数を有する。
重力:FG=ρsVg
浮力:Fb=ρVg
ここで、ρs、ρは堆積物、流体の密度であり、Vは堆積粒子の体積、gは重力加速度である。
1) ナノ粒子の高い添加濃度は分散を改善し;
2) ビヒクルの粘度の増大は分散を改善し;
3) より小さな粒径のナノ粒子はより長時間懸濁する。
1)長期間の分散を達成するためには、ナノ粒子の体積添加濃度を増大させることが有用な方法である可能性がある。
2)ナノ粒子の高い添加濃度を用いれば、50nmのナノ粒子に対しては良好な分散液を得ることができる。
3)ビヒクルの粘度を増大させることは速度の低下をもたらす。
この「排除」体積は、フレキシブルなアルキル(またはエトキシ)鎖によって「占有されている」空間を表し、それは第二の銅ナノ粒子によって占有されることのあり得ない空間である。この「排除」体積が大きいほど、該分散剤は銅ナノ粒子の分離された状態を保つのにより効果的である。この「排除」体積の第二の態様は、大きな値が、低濃度の化合物がナノ粒子の高レベルの被覆と、それ故、分散剤としての高度の有効性とを提供するのに効果的であることを可能にすることである。
酸性基を有するコポリマーを分散剤として用い、相溶性ビヒクルと共に銅インクを配合する。イオン性の基を有するコポリマー、例えば、ディスパービック(Disperbyk)180、ディスパービック111、スチレン無水マレイン酸コポリマー(SMA1440フレーク)、PT、HCS−P、HCS−N等は、イオン性のものであり、そのため静電的分散を得ることができる。2−ブトキシエチルアセテート、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、エチレングリコールブチルエーテル、シクロヘキサノン、シクロヘキサノール、2−エトキシエチルアセテート、エチレングルコールジアセテート、テルピネオール、イソブチルアルコール等の相溶性ビヒクルのいずれか1つまたはそれらの組み合わせを用いて、銅ナノ粒子と共に銅インクを配合することができる。その銅インクはフレキシブル基板上にインクジェット印刷される。次いで、前硬化プロセスを用いて、空気中150℃未満の低温でビヒクルおよび分散剤にあたるものを除去する。最後に、印刷された銅インクに光焼結を適用して、銅ナノ粒子を溶融して導体にする。分散剤の重量百分率は0.5%から20%の範囲であり得る。銅ナノ粒子の添加濃度は10%から最大60%までであり得る。
より良好な分散を得るために、非イオン性分散剤およびイオン性分散剤の両方を用いて銅インクを配合する。非イオン性分散剤、例えば、トリトンX−100、トリトンX−15、トリトンX−45、トリトンQS−15、線状アルキルエーテル(colar Cap MA259、colar Cap MA1610)、四級化アルキルイミダゾリン(Cola Solv IES、Cola Solv TES)、ポリビニルピロリドン(PVP)等、および、イオン性の基を有するコポリマー、例えば、ディスパービック180、ディスパービック111等、ならびに、スチレン無水マレイン酸コポリマー(SMA1440フレーク)、PT、HCS−P、HCS−N等を銅インクと配合することができる。銅酸化物により不動態化された銅ナノ粒子を配合に用いる。相溶性ビヒクル、例えば、2−ブトキシエチルアセテート、プロピレングリコールモノメチルエーテルアセテート、ジエチレングリコールモノエチルエーテルアセテート、2−エトキシエチルアセテート、エチレングリコールジアセテート、エチレングリコールブチルエーテル、シクロヘキサノン、シクロヘキサノール等、を選択して、銅ナノ粒子と共に銅インクを配合することができる。特に、2−ブトキシエチルアセテートとプロピレングリコールモノメチルエーテルアセテートとの組み合わせ、2−エトキシエチルアセテートと2−エトキシエチルアセテートとの組み合わせ、およびエチレングリコールジアセテートとプロピレングリコールモノメチルエーテルアセテートとの組み合わせが、イオン性分散剤および非イオン性分散剤の両方と相溶性であるので使用することができる。分散剤の重量百分率は、0.5%から20%の範囲であり得る。銅ナノ粒子の添加濃度は10%から最大60%までであり得る。
光焼結により高純度銅膜を得るためには、少ない有機残留物が高導電率をもたらす。沸点の低いビヒクルおよび分散剤が銅インクを配合するために選択される。分散剤の重量百分率は0.5%から20%の範囲であり得る。銅ナノ粒子の添加濃度は10%から最大60%までであり得る。低沸点のアルコールまたは他の溶媒、例えば、イソプロピルアルコール、エタノール、トルエン、ブチルベンゼンおよび水等、をビヒクルとして用いることができる。比較的低い分子量を有する低沸点アミン、例えば、ヘキシルアミン、オクチルアミン等、をインク配合用の分散剤として用いることができる。これらの低沸点ビヒクルおよびアミンは、前硬化プロセスが150℃未満の低温でコートされたインクに適用されるとき、容易に蒸発させることができる。アミンは、それらのほとんどが前硬化プロセス中に蒸発するように、150℃未満の低い沸点を有するべきである。前硬化段階は、印刷されたまたはコートされた金属ナノ粒子が、それらが光焼結される前に乾燥していることを確保するために必要である。この段階は、150℃未満の空気中で行われる。この段階が必要なのは、光焼結すべき金属ナノ粒子が揮発性の化合物を含有する場合、光硬化中の急速加熱がその化合物の非常に急速な蒸発を生じさせて、金属ナノ粒子のコートされた膜が不連続で非常に粗い表面となるプロセスが得られるためである。
銅インクは、低コストの堆積技法、例えば、スプレー、ドローダウン、スピンキャスティング等、のために配合される。その銅インクは、銅ナノ粒子、ビヒクル、分散剤を含む。ビヒクルは、イソプロピルアルコール(IPA)、トルエン、ブチルベンゼンまたは水等であり得る。アミン(例えばヘキシルアミン)が、銅ナノ粒子用の分散剤として使用される。銅ナノ粒子の大きさは、2nmから200nmまでの範囲である。銅の添加濃度は10%から50%までであり得る。分散剤の添加濃度はインク中に1%から30%までであり得る。該銅インクは、ドローダウン法を用いて、ポリイミド基板上に堆積される。硬化前の銅膜の厚さは1μmから10μmまでであり得る。その銅膜は、光硬化の前に、空気中100℃で30分間前硬化される。前硬化された膜は絶縁性であり、抵抗率は2×107Ωを超える。
図24Aは、半導体産業において用いられる石英プレート上に作製した標準的なフォトマスクを示す。暗色領域は、高エネルギー光を通過させることのできる開口部であり、残りの領域は、受け取った高エネルギー光を反射および吸収する金属膜がコートされている。フォトマスクの開口部を通って受け取られた高エネルギー光は、基板上の銅インクを選択的に焼結させ、銅インクの他の領域は高エネルギー光に露光されないままに残す。銅インクの露光領域は、融合してポリイミド基板に接着し、非露光領域は基板に対する接着性が非常に弱い。図24Bは、銅インクの非露光領域を、水または他の溶媒で洗い流すことによって、あるいは単純にテープによって除去された後に、フォトマスクに対応する正確にパターン化された銅膜が得られ、その使用されたフォトマスクによって画定された銅トレースと同じ解像度が得られることを示している。これは、銅パターンの解像度がフォトマスクの解像度に依存することを実証している。
図25Aは、カプトン膜から作られたシャドーマスクを示す。白色領域はカプトン基板の開口部であり、高エネルギー光を通過させる。そのカプトン膜は、いくらかのUV光、可視光および赤外光を吸収し、そのためその通過光はナノ粒子を焼結させるのに十分なエネルギーを有さず、一方で、開口部を通過する高エネルギー光は、ナノ粒子を焼結させるのに十分なエネルギーを有する。図25Bは、非焼結領域を水または溶媒で洗い流すかまたはテープによって除去した後に、カプトンシャドーマスクに対応するパターン化された銅膜が得られることを示している。
1)高導電性マイクロ構造体の直接記録は、何らのフォトリソグラフィー処理も必要としない。残留する未処理物質は容易に取り除くことができる。
2)電気メッキ銅に対して広範に用いられているシード層を必要としない。
3)この付加的なマイクロリソグラフィー技法は安価であり(フォトリソグラフィーを必要としない)、高い処理能力である。マイクロおよびサブマイクロ構造体を、大気中で高速位置決めシステムおよび走査性レーザービームを用いることによって、予定位置に直接作ることができる。
4)導電性3Dマイクロ構造体は、何らのフォトリソグラフィー処理も用いずに、層毎の処理で構築可能である。
1)電気メッキ法では、高アスペクト比でビアを充填するのに時間がかかり得る。
2)銅の電気メッキ用のバリア/シード層を堆積するためPVD設備を、高アスペクト比のビアの一様なコーティングを有するように開発しなければならない。
3)ビアを充填するため、化学薬品および添加剤を改良する必要がある。化学添加剤の消費量も重要である。
4)銅トレースを作製するのに、フォトリソグラフィー処理が必要である。
10〜40μm、50〜100μmの深さ、20〜50μmの間隔の範囲でビア開口部を充填することが、半導体産業によって現在追求されている。より小さな模様もまた必要であり得る。現状では、TSV技術での主な挑戦は、これを如何にして高い生産性でコスト効率的に作製し、ボイド無しにビアを充填し、良好な電気的結果を獲得するかということである。
102 基板
104 プリンター装置
106 貯蔵区画
300 ナノ粒子
302 金属酸化物層を有する金属
304 金属酸化物層
306 アルコール
800 装置
801 銅インク
802 インクジェットディスペンサ
803 インク膜
804 基板
805 パターンアウトライン
806 光源
807 ミラー
808 コンピュータ/制御装置
809 導電性膜
1000 銅ナノ粒子インク
1002 基板
1004 マスク
1005 透明プレート
1006 金属パターン
1008 導電性膜
1010 非導電性膜
1100 繊維
1102 スプール
1104 インクバス
1106 コートされた繊維
1108 乾燥器
1110 乾燥されたインクがコートされている繊維
1112 光焼結ステーション
1114 光焼結された繊維
1116 繊維巻取りスプール
Claims (17)
- 2つ以上の酸素化された有機化合物を含むビヒクルと、
銅ナノ粒子と、
150℃未満の低い沸点を有するイオン性分散剤と、
中鎖脂肪族アルコールと、
を含み、
前記中鎖脂肪族アルコールが、4個と12個を含めて4個から12個までの炭素原子を有し、
前記中鎖脂肪族アルコールの粘度が、前記ビヒクルの粘度を上回り、
前記ビヒクルの沸点が、150℃未満であり、
前記銅ナノ粒子が、酸化銅を含む導電性金属インク。 - 前記アルコールが、イソブタノール、2−オクタノール、またはそれらの組合せである、請求項1に記載のインク。
- 前記アルコールの誘電率が、前記ビヒクルの誘電率を上回る、請求項1に記載のインク。
- 前記アルコールが、非ポリマーアルコールである、請求項1に記載のインク。
- 前記アルコールが、インク中の有機液体の約30重量%から約96重量%の間である、請求項1に記載のインク。
- 前記イオン性分散剤が、前記インクの約0.5重量%から20重量%の間を構成する、請求項1に記載のインク。
- 前記銅ナノ粒子が、前記インクの約40重量%から約60重量%の間を構成する、請求項1に記載のインク。
- 前記ビヒクルが、親水性である、請求項1に記載のインク。
- 前記インクが、バインダーを含まない、請求項1に記載のインク。
- 前記インクが、直径約10μmより大きいナノ粒子の凝集物を実質的に含まない、請求項1に記載のインク。
- 前記インクが、硬化して平坦で均質な導体を形成することができる、請求項1に記載のインク。
- 金属インクから導体を形成する方法であって、
金属インクを基板上に堆積して前記基板上に平坦で均質なインクの層を形成する段階であり、前記インクが、
2つ以上の酸素化された有機化合物を含むビヒクルと、
銅ナノ粒子と、
150℃未満の低い沸点を有するイオン性分散剤と、
中鎖脂肪族アルコールと、
を含む段階と、
前記導電性金属インクを凝固させて前記基板上に導体を形成する段階と、
を含み、
前記中鎖脂肪族アルコールが、4個と12個を含めて4個から12個までの炭素原子を有し、
前記中鎖脂肪族アルコールの粘度が、前記ビヒクルの粘度を上回り、
前記ビヒクルの沸点が、150℃未満であり、
前記銅ナノ粒子が、酸化銅を含む方法。 - 前記インクが、直径約10μmより大きいナノ粒子の凝集物を実質的に含まない、請求項12に記載の方法。
- 堆積段階が、ドローダウン印刷を含む、請求項12に記載の方法。
- 堆積段階が、インクジェット印刷を含む、請求項12に記載の方法。
- 前記導体の抵抗率が、約10μΩ・cm未満である、請求項12に記載の方法。
- 前記銅ナノ粒子が、前記インクの約40重量%から約60重量%を構成する、請求項12に記載の方法。
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US12/415,761 US8404160B2 (en) | 2007-05-18 | 2009-03-31 | Metallic ink |
PCT/US2010/028799 WO2010114769A1 (en) | 2009-03-31 | 2010-03-26 | Metallic ink |
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EP (1) | EP2414109B1 (ja) |
JP (1) | JP5957630B2 (ja) |
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EP2414109B1 (en) | 2020-04-29 |
KR101777311B1 (ko) | 2017-09-15 |
TW201544557A (zh) | 2015-12-01 |
TW201103960A (en) | 2011-02-01 |
JP2012522114A (ja) | 2012-09-20 |
US8404160B2 (en) | 2013-03-26 |
CN102448623B (zh) | 2016-01-20 |
KR20120050924A (ko) | 2012-05-21 |
TWI494384B (zh) | 2015-08-01 |
US20090274833A1 (en) | 2009-11-05 |
EP2414109A1 (en) | 2012-02-08 |
TWI612106B (zh) | 2018-01-21 |
CN102448623A (zh) | 2012-05-09 |
WO2010114769A1 (en) | 2010-10-07 |
EP2414109A4 (en) | 2014-10-01 |
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