JP6959977B2 - 高導電性銅パターンを製造するための調合物および方法 - Google Patents
高導電性銅パターンを製造するための調合物および方法 Download PDFInfo
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- JP6959977B2 JP6959977B2 JP2019501665A JP2019501665A JP6959977B2 JP 6959977 B2 JP6959977 B2 JP 6959977B2 JP 2019501665 A JP2019501665 A JP 2019501665A JP 2019501665 A JP2019501665 A JP 2019501665A JP 6959977 B2 JP6959977 B2 JP 6959977B2
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Description
[1] Lee et al., J. Mater.Chem. 2012, 22, 12517-12522
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[9] PCT 国際公開 WO 2012/077548
[10] PCT 国際公開 WO 2009/098985
[11] 米国特許公開 US 8,801,971
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[13] Copper and Copper Alloys, Joseph R. Davis, ASM International 2001, pp. 181, 297
導電性パターンは、様々な印刷方法で面上に導電性インクを印刷することによって得られる。使用される一般的な導電性インクの中には、銀粒子をベースとするインク調合物があり、これは十分に高い導電性を提供するが、そのようなインクは依然として比較的高価であり、従って大規模生産の一部としての利用には問題がある。銅は、その高い導電性と比較的低コストのために、高導電性の印刷パターンを得るための潜在的な材料として広く研究されてきた。導電性パターンを得るための方法の1つは、金属を印刷することを含み、これは、銅ナノ粒子または銅前駆体を基材上に形成し、続いてナノ粒子または前駆体を焼結または熱分解して、連続した金属パターンを得る[1−4]。当技術分野で知られているように、焼結は、物質の個別の粒子を加熱して粒子の固体または実質的に連続した塊への固体拡散駆動接合を引き起こす(すなわち、プロセス中に粒子の溶融および/または液化がない)プロセスである。
(a)液体キャリア中に銅ナノ粒子を含む分散液またはペーストを、基材の少なくとも表面領域上に適用するステップと、
(b)少なくとも1つの銅酸化剤を適用するステップと、
(c)Cu0をCuHに変換するために銅ナノ粒子の少なくとも一部を前記銅酸化剤と反応できるようにし、それによって基材上にインク調合物のパターンを得るステップとを含む。
(i)液体キャリア中に銅ナノ粒子を含む分散液またはペーストを、基材の少なくとも表面領域上に印刷するステップと、
(ii)少なくとも1つの銅酸化剤を前記基材に適用するステップと、
(iii)Cu0をCuHに変換するために、銅ナノ粒子の少なくとも一部を前記銅酸化剤と反応させることにより、パターン担持基材を得るステップと、
(iv)CuHの分解および銅の焼結を可能にする条件に前記パターン担持基材をさらすステップとを含み、当該さらすステップは、約0.01から600秒の間の期間であり、それによって導電性銅パターンを得る。
シングルステップ印刷インク調合物
銅NP分散液を限外濾過膜(CO=100KDa、PES)で洗浄した。いくつかの調合物では、水を様々な液体キャリアと交換して、液体キャリア中に30〜60重量%の銅を有する調合物を得た。得られた赤色インクは、1μmシリンジフィルタを通して容易に濾過された。表1に詳述されるように、シングルステップ印刷に適した調合物を得るために次亜リン酸(HPA)を混合物に添加した。
30重量%の銅を含む実施例1.1のジプロピレングリコールメチルエーテル系分散液を、0.08の重量比(銅/HPA)でHPAと混合した。インク調合物をDMCdimatixインクジェットヘッドを用いてインクジェット印刷した。印刷は安定しているようにみえた。得られたパターンを大気雰囲気中で300℃で焼成し、抵抗値を測定した。(得られた線形プロファイルにより)抵抗率を計算すると、7μΩ×cmとなり、これは銅バルク導電率の24%に等しい。XRD分析は、酸化物なしで得られたパターンにおいて100%のfcc銅を示した。
2ステップ印刷では、まず、実施例1.1に記載の合成によって得られた銅ナノ粒子のキャリア液中の分散液を基材に印刷してパターンを得た。パターンは、数秒から数分までの間、20〜150℃の温度で乾燥された。
ジプロピレングリコールメチルエーテル中の10重量%HPA溶液を、予め印刷された銅NPパターン上にインクジェット印刷した。次いで、パターンを空気中で10秒間140℃に加熱した。0.05〜1Ω(オーム)の抵抗が1cmの線に沿って測定された。
銅NPの印刷パターンを50重量%のHPA/水溶液中に1〜10秒間浸漬した。次いで、パターンを水中で1分まで洗浄し、そして60〜150℃で5〜60秒間乾燥させた。その後、パターンを空気中125〜500℃の温度で1秒〜20分間焼結した。図1は、紙に印刷され、次いで50重量%HPAに5秒間浸漬され、水で30秒間洗浄され、次いで空気中で60秒間焼結された液体分散インク調合物についての焼結温度の関数としての電気抵抗の変化を示す。理論に束縛されることを望まないが、120℃より高い焼結温度で、CuHが分解して局所的にH2雰囲気を形成し、それが酸化銅の形成を妨げ、焼結のための金属間相互作用を可能にする。
銅NP印刷パターンを50重量%HPA/水溶液と共に容器に入れ、20〜130℃に加熱した。温度が上昇するにつれて、多くのHPA蒸気が形成され、その結果、CuHを得るために必要とされる暴露時間が短くなる。曝露時間は10秒〜3時間の範囲内であった。
・焼結温度の影響
上記のように、図1は、異なる焼結温度で得られた焼結銅パターンの%バルク導電率を示す。全てのサンプルを空気中で60秒間焼結した。図示のように、少なくとも20%のバルク導電率の値が得られ、そしてこれは焼結温度の増加と共に増加したが、これはCuHの熱分解の速度および程度の増大によるものと思われる。
図2は、空気中150℃の一定温度での様々な期間の焼結を示す。図2から明らかなように、%バルク導電率の有意な変化は経時的に観察されなかったので、焼結は数秒以内に起こる(150℃への暴露で2秒)。酸化銅の分解には高温(150℃以上、典型的には約250〜300℃)および著しく長い焼結時間(少なくとも1時間)が必要とされるので、これはまた、酸化銅の形成および分解を伴わない焼結のメカニズムが証明された。
実施例1に従って調製された60重量%Cuペーストで得られた抵抗率に対するHPA/Cu重量比の影響を評価した。
湿度85%、85℃での耐久性試験の結果は、焼結パターンが安定であることを明らかにした。何のコーティングもしなければ、抵抗率は408時間後に44%増加し、シーラント層を有する場合には26%増加した。これらの結果は、本開示の調合物および方法から得られた焼結パターンが非常に安定であり、極端な条件にさらされた後でも非常に高い導電率が維持されたことを示している。
本開示の調合物の近赤外(NIR)焼結も評価された。800Wのランプを使用して表1の例3および4に従って調製した試料を焼結した。試料を0.5〜5秒間NIRランプに露光し、0.07Ω/sqまでのシート抵抗を得た。
実施例1の配合#16に記載のペーストを、スクリーン印刷により種々の基材上に印刷して導電線を形成した。
(a)紙
(b)シリコンウエハ
(c)ITOコーティングしたシリコンウェハ
(d)ITOコーティングガラス
(e)カプトン(ポリイミドフィルム)
4.1 RFIDアンテナ:実施例3に記載したようにE52RFIDアンテナを紙に印刷した。次に、チップをアンテナに取り付け、アンテナの性能を特徴付けた。アンテナ性能は、約−6.5dBmにエッチングされたアンテナの性能に匹敵することが分かった。図6は、紙に印刷されたそのようなE52アンテナの写真を示す。
焼結パターン中の蛍光体を検出するために、EDX分析を行った。分析は、配合#21(表1)によって印刷され、150℃で30秒間焼結されたパターンについて行われた。
Claims (15)
- 銅ナノ粒子と、銅酸化剤としての次亜リン酸(hypophosphorous acid)(HPA)と、CuHとを含むことを特徴とするインク調合物。
- 請求項1のインク調合物において、少なくとも0.0001重量%のCuHを含むことを特徴とするインク調合物。
- 請求項1のインク調合物において、前記調合物が約10〜90重量%の銅ナノ粒子を含むことを特徴とするインク調合物。
- 請求項1のインク調合物において、前記調合物が前記銅酸化剤を約0.001〜20重量%含むことを特徴とするインク調合物。
- 請求項1のインク調合物において、前記銅酸化剤と前記銅ナノ粒子との間の比率が、約0.001〜約0.2(重量/重量)であることを特徴とするインク調合物。
- 請求項1のインク調合物において、分散液またはペーストの形態であることを特徴とするインク調合物。
- 請求項1のインク調合物を調製するためのキットであって、液体キャリア中に銅ナノ粒子の分散液またはペーストを含む第1の容器と、
銅酸化剤としての次亜リン酸(hypophosphorous acid)(HPA)の溶液を含む第2の容器と、を含むことを特徴とするキット。 - 請求項1のインク調合物を含むことを特徴とする印刷パターン。
- 基材上にパターンを得る方法であって、
(a)液体キャリア中に銅ナノ粒子を含む分散液またはペーストを、基材の少なくとも表面領域上に適用するステップと、
(b)銅酸化剤としての次亜リン酸(hypophosphorous acid)(HPA)を適用するステップと、
(c)Cu0をCuHに変換するために銅ナノ粒子の少なくとも一部を前記銅酸化剤と反応できるようにし、それによってインクのパターンを得るステップとを含むことを特徴とする方法。 - 請求項9の方法において、ステップ(b)がステップ(a)の前に行われることを特徴とする方法。
- 導電性銅パターンを基材上に得るための方法であって、
請求項1に記載のインク調合物を前記基材の少なくとも表面領域上に印刷してパターン担持基材を得るステップと、
前記パターン担持基材を、CuHの分解および銅の焼結を可能にする条件にさらすステップとを含み、当該さらすステップは、約0.01から600秒の間の期間であり、それによって導電性銅パターンを得ることを特徴とする方法。 - 導電性銅パターンを基材上に得る方法であって、
(i)液体キャリア中に銅ナノ粒子を含む分散液またはペーストを、基材の少なくとも表面領域上に印刷するステップと、
(ii)銅酸化剤としての次亜リン酸(hypophosphorous acid)(HPA)を前記基材に適用するステップと、
(iii)Cu0をCuHに変換するために、前記銅ナノ粒子の少なくとも一部を前記銅酸化剤と反応させることにより、パターン担持基材を得るステップであって、このパターンは請求項1のインク調整物を含むステップと、
(iv)CuHの分解および銅の焼結を可能にする条件に前記パターン担持基材をさらすステップとを含み、当該さらすステップは、約0.001から600秒の間の期間であり、それによって導電性銅パターンを得ることを特徴とする方法。 - 請求項12の方法において、CuHの分解および銅の焼結を可能にする条件が、前記パターンを有する基材を少なくとも125℃の温度にさらすことを含むことを特徴とする方法。
- 請求項12の方法によって得られることを特徴とする、少なくとも5%の%バルク導電率を有する導電性銅パターン。
- 請求項12の方法によって得られることを特徴とする、実質的に酸化銅を含まない導電性銅パターン。
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KR101697097B1 (ko) * | 2014-12-23 | 2017-01-18 | 전자부품연구원 | 나노구리 잉크 조성물, 그를 이용한 배선기판 및 그의 제조 방법 |
EP3099146B1 (en) * | 2015-05-27 | 2020-11-04 | Agfa-Gevaert | Method of preparing a silver layer or pattern comprising a step of applying a silver nanoparticle dispersion |
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KR102397518B1 (ko) | 2022-05-13 |
EP3494184A1 (en) | 2019-06-12 |
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