JP7137862B2 - 貴金属被覆銀ナノワイヤー、コーティングを行うための方法および安定化透明導電性フィルム - Google Patents
貴金属被覆銀ナノワイヤー、コーティングを行うための方法および安定化透明導電性フィルム Download PDFInfo
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- JP7137862B2 JP7137862B2 JP2020138079A JP2020138079A JP7137862B2 JP 7137862 B2 JP7137862 B2 JP 7137862B2 JP 2020138079 A JP2020138079 A JP 2020138079A JP 2020138079 A JP2020138079 A JP 2020138079A JP 7137862 B2 JP7137862 B2 JP 7137862B2
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Description
本出願は、両方とも“Noble Metal Coated Silver Nanowires,Methods for Performing the Coating and Stabilized Transparent Conductive Films”と題された、Huらに対する2015年8月11日に出願された係属中の米国特許出願第14/823,001号明細書、およびHuらに対する2015年4月3日に出願された米国仮特許出願第62/142,870号明細書の(両方とも参照によって本願明細書に組み込まれる)優先権を主張する。
被覆銀ナノワイヤーは、コーティングのための適切な合成手法によるコーティングの検鏡により平滑に見え得る貴金属コーティングを有する。処理は、堆積される貴金属の量を変更するように調整することができる。改良されたコーティング方法に基づいて、直接貴金属堆積またはガルバニック置換が、平滑な貴金属コーティングを堆積するのに使用され得る。一般的には、貴金属コーティングは、コーティングを形成する貴金属堆積を加減する選択されたリガンドを用いて、ならびに他の反応剤および加工条件の適切な選択(反応剤の適切な徐々の添加など)によって制御することができる。貴金属の還元の制御は、望ましく平滑および均一なコーティングの形成を促進することが判明した。本明細書に記載されるように、貴金属被覆銀ナノワイヤーは、透明導電性フィルムの形成のためのすぐれた材料を提供する。
透明な電気導電性構造物またはフィルムは一般的に、光学的性質を著しく好ましくない方向に変えずに電気導電率を提供する薄く広がった金属導電層と、導電性要素の機械的支持ならびに保護を提供する様々な付加的な層とを含む。薄く広がった金属導電層は非常に薄く、相応して機械的誤用およびその他の誤用によって損傷を受けやすい。基材の構造内に1つまたは複数の層を有することができる基材上に薄く広がった金属導電層を形成することができる。基材は一般的に、自立フィルムまたはシート構造として扱うことができる。アンダーコートと称される、薄い溶液加工層を任意選択により基材フィルムの上面に沿っておよび薄く広がった金属導電層のすぐ下に置くことができる。また、基材の反対側の薄く広がった金属導電の面に特定の保護をもたらす付加的な層で薄く広がった金属導電性層をコートすることができる。一般的には、電気導電性構造物を最終製造物においてどちらかの向きに置くことができ、すなわち、基材の外側に向いている基材が電気導電性構造物を支持する製造物の表面に接している。
薄く広がった金属導電層は一般的に、金属ナノワイヤーから形成される。十分な添加量および選択されるナノワイヤーの性質によって、相応する適切な光学的性質を有するナノワイヤーを使用して適度の導電率を達成することができる。本明細書に記載された安定化されたフィルム構造物が様々な薄く広がった金属導電性構造物を有するフィルムの望ましい性能をもたらすことができることが予想される。しかしながら、特に望ましい性質は融着金属ナノ構造ネットワークによって達成された。
融着金属ナノ構造ネットワークは、良い光学的性質を提供しながら低い電気抵抗を提供することができる。したがって、フィルムは透明導電性電極等として有用であり得る。透明導電性電極は、太陽電池の受光表面に沿う電極などの様々な用途に適し得る。ディスプレイのためにおよび特にタッチスクリーンのために、フィルムをパターン化して、フィルムによって形成される電気導電性パターンを提供することができる。パターン化フィルムを有する基材は一般的に、パターンの各部分において良い光学的性質を有する。
使用の際、透明導電性フィルムが、対応するデバイスの耐用年数などの商業的に受け入れられる時間、持続することが望ましい。薄く広がった金属導電層は、適切な試験下で、薄く広がった金属導電層の導電性の維持について評価され得る。性能を試験するために、加速エージング手順は、妥当な期間にわたって客観的な評価を提供するのに使用され得る。これらの試験は、市販の環境試験装置を用いて行われ得る。
本明細書に説明された透明導電性フィルムを、多くの電子デバイスに使用されるタッチスクリーンに適合し得るタッチセンサーに有効に組み込むことができる。いくつかの代表的な実施形態が一般的にここで説明されるが、透明導電性フィルムを他の所望の設計に適合させることができる。タッチセンサーの一般的な特徴は一般的に、自然な状態で、すなわち、触れられたあるいは他の方法で外的に接触されない時に離隔された配置の2つの透明導電性電極構造物の存在である。キャパシタンスに基づいて作動するセンサーについては、誘電体層は一般的に2つの電極構造物の間にある。図3を参照して、代表的なキャパシタンスに基づいたタッチセンサー202が、ディスプレイ成分204と、任意選択の下部基材206と、第1の透明導電性電極構造物208と、誘電体層210、例えばポリマーまたはガラス板と、第2の透明導電性電極構造物212と、任意選択の上蓋214と、センサーに触れることと関連づけられたキャパシタンスの変化を測定する測定回路216とを含む。図4を参照して、代表的な抵抗に基づいたタッチセンサー240が、ディスプレイ成分242と、任意選択の下基材244と、第1の透明導電性電極構造物246と、第2の透明導電性電極構造物248と、それらの自然な構成において電極構造物の離隔された構成を支持する支持体構造物250、252と、上側覆い層254と抵抗測定回路256とを含む。あるいは、センサーは、透明導体の2つの層(支持体および誘電体層の両方として働く基材(プラスチックまたはガラス)の各表面に1つずつ)を備えた1つの単一のフィルムから構成され得る。センサーはまた、透明導電性材料の単一の層から構成され得、ここで、より正確なパターン化および加工が、「X」および「Y」導電性要素を空間的に分けるのに必要とされる。
貴金属被覆NWベースの透明導体はまた、タッチセンサーに加えて、様々な他の用途に用いられ得る。特に、向上した電気化学的安定性、熱安定性、および向上した酸化安定性により、これらの材料は、エレクトロクロミック、PDLC(高分子分散型液晶)デバイスおよびフィルムなどの用途において透明導体としてよく適している。非被覆AgNWと比較して、貴金属被覆NWのより広い範囲の化学的適合性および全体的な耐久性は、これらの(被覆)材料が、以下の用途によく適し得ることも示す:光起電、スマートウィンドウ、エレクトロクロミック、OLED(照明およびディスプレイ)、電気化学および生化学センサー用の安定した電極。
この実施例は、ガルバニック置換を用いて、銀ナノワイヤーの有効なコーティングを実証する。イソプロパノール中のAgナノワイヤーの分散体(1重量%、100mL)を、300mLの脱イオン水と混合し、沸騰するまで加熱した(約85℃)。磁気撹拌下で沸騰混合物に、350mLの脱イオン水、0.75mLの塩化白金酸溶液(H2PtCl6、0.1M)および0.2mLのエチレンジアミンから構成されるPt成長溶液を、200~800μL/分の速度で滴下して加えた。添加の後、混合物を室温に冷まし、Pt被覆Agナノワイヤーを、アセトンの添加による沈殿、続いて遠心分離、脱イオン水によるすすぎによって3回精製し、精製の後、100mLのイソプロパノール中で再度分散させた。代表的な被覆ナノワイヤーのTEM顕微鏡写真が、図5B(より低い倍率)および6B(より高い倍率)に示される。代表的な被覆ナノワイヤーの組成のEDS測定が、図7A~7Eに示される。図7Aは、EDS定量線走査についての区切られた領域を有する被覆ナノワイヤーのTEM画像を示す。図7Bおよび7Cはそれぞれ、銀原子パーセントおよび白金原子パーセントの評価の画像を示す。相応して、図7Dおよび7Eはそれぞれ、白金および銀についてナノワイヤー断面にわたって走査された原子パーセントのプロットである。
この実施例は、直接堆積を用いた白金による銀ナノワイヤーの有効なコーティングを実証する。イソプロパノール中の銀ナノワイヤーの分散体(1重量%、360g)を、1380mLの脱イオン水と混合した後、40mLのポリビニルピロリドン(PVP)水溶液(5重量%)および0.9mLのヒドラジン溶液(35重量%)を加えた。160mLの脱イオン水、16mLのPVP水溶液(5重量%)、9.6mLの亜硝酸ナトリウム水溶液(NaNO2、1M)および1.6mLの塩化白金酸溶液(H2PtCl6、0.1M)から構成される白金(Pt)前駆体混合物を、200~800μL/分の速度で滴下して加えた。磁気撹拌をプロセス全体にわたって維持した。最終生成物を、アセトン沈殿および遠心分離の後それぞれ、脱イオン水で3回洗浄し、洗浄されたナノワイヤーを、360gのイソプロパノール中で再度分散させる。代表的な被覆ナノワイヤーのTEM顕微鏡写真が、図5C(より低い倍率)および6C(より高い倍率)に示される。代表的な被覆ナノワイヤーの組成のEDS測定が、図8A~8Eに示される。図8Aは、EDS定量線走査について区切られた領域を有する被覆ナノワイヤーのTEM画像を示す。図8Bおよび8Cはそれぞれ、銀原子パーセントおよび白金原子パーセントの評価の画像を示す。相応して、図8Dおよび8Eはそれぞれ、白金および銀についてナノワイヤー断面にわたって走査された原子パーセントのプロットである。
この実施例は、ガルバニック置換を用いた金による銀ナノワイヤーの有効なコーティングを実証する。イソプロパノール中のAgナノワイヤーの分散体(1重量%、100mL)を、300mLの脱イオン水と混合し、沸騰するまで加熱した(約85℃)。磁気撹拌下で沸騰混合物に、350mLの脱イオン水、0.3mLのクロロ金酸(HAuCl4、0.25M)、および0.2mLのエチレンジアミンから構成されるAu成長溶液を、200~800μL/分の速度で滴下して加えた。添加の後、混合物を室温に冷まし、Au被覆Agナノワイヤーを、アセトンによる沈殿、遠心分離、続いて脱イオン水による洗浄によって3回精製し、洗浄されたナノワイヤーを、100mLのイソプロパノール中で再度分散させた。代表的な被覆ナノワイヤーのTEM顕微鏡写真が、図5D(より低い倍率)および6D(より高い倍率)に示される。代表的な被覆ナノワイヤーの組成のEDS測定が、図9A~9Eに示される。図9Aは、EDS定量線走査について区切られた領域を有する被覆ナノワイヤーのTEM画像を示す。図9Bおよび9Cはそれぞれ、銀原子パーセントおよび白金原子パーセントの評価の画像を示す。相応して、図9Dおよび9Eはそれぞれ、白金および銀についてナノワイヤー断面にわたって走査された原子パーセントのプロットである。
この実施例は、白金コーティング厚さに応じた被覆ナノワイヤーの性質の検査を提供する。
この実施例は、ポリエステル基材上にナノ構造ネットワークを形成する貴金属被覆銀ナノワイヤーの能力を実証する。
この実施例は、透明導電性フィルムにおける貴金属被覆銀ナノワイヤーの向上した熱安定性を実証する。
この実施例は、様々なPt厚さのPt被覆銀ナノワイヤーで作製されたフィルムの光安定性を試験する。
この実施例は、高湿度および高温条件下で、透明導電性フィルムにおける貴金属被覆銀ナノワイヤーの向上した安定性を実証する。
この実施例は、85℃の条件下で、フィルムにおける貴金属被覆銀ナノワイヤーの安定性を試験する。
この実施例は、透明導電性フィルムにおける貴金属被覆銀ナノワイヤーの電気化学的(またはレドックス)安定性を試験する。
Claims (15)
- 直接金属堆積によって貴金属被覆銀ナノワイヤーを形成するための方法であって、
溶解された貴金属イオンおよび金属イオン錯化リガンドを含むコーティング溶液を、銀ナノワイヤーおよび還元剤を含む反応溶液中に少なくとも15分にわたって徐々に加えて、前記銀ナノワイヤー上に貴金属コーティングを形成する工程、および
1nm以下の二乗平均平方根粗さを有する貴金属被覆銀ナノワイヤーを取得する工程、を含む方法。 - 前記金属イオン錯化リガンドが、ニトライト(nitrite)、ジエチルアミン、エチレンジアミン、ニトリロ三酢酸、イミノビス(メチレンホスホン酸)、アミノトリス(メチレンホスホン酸)、エチレンジアミン四酢酸(EDTA)、1,3-プロピレンジアミン四酢酸(1,3-PDTA)、トリエチレンテトラミン、トリ(2-アミノエチル)アミン、ジエチレントリアミン五酢酸、1,2-シクロヘキサンジアミノ四酢酸、イミノ二酢酸、メチルイミノ二酢酸、N-(2-アセトアミド)イミノ酢酸、N-(2-カルボキシエチル)イミノ二酢酸、N-(2-カルボキシメチル)イミノジプロピオン酸、ピコリン酸、ジピコリン酸、ヒスチジン、それらの組合せからなる群から選択される、請求項1に記載の方法。
- 前記コーティング溶液が、貴金属イオン当たり少なくとも2のリガンドのモル比を有する、請求項1または2に記載の方法。
- 前記反応溶液が、キャッピングポリマーをさらに含み、ここで、前記コーティング溶液が、0.0001M~5Mの貴金属イオンを含み、前記反応溶液が、0.02重量%~3.5重量%の銀ナノワイヤー、0.01重量%~1.5重量%のキャッピングポリマーおよび1マイクロモル~1ミリモルの還元剤を含む、請求項1~3のいずれか一項に記載の方法。
- 前記貴金属被覆銀ナノワイヤーが0.05重量%~15重量%の貴金属を有する、請求項1~4のいずれか一項に記載の方法。
- ガルバニック交換によって貴金属被覆銀ナノワイヤーを形成するための方法であって、
貴金属イオンと錯化リガンドとの混合物を含むコーティング溶液を、銀ナノワイヤーとキャッピングポリマーとの分散されたブレンドを含む加熱された反応溶液に少なくとも1時間にわたって徐々に加えて、銀を貴金属に徐々に置き換えて、貴金属コーティングを備えた無傷の銀コアを形成する工程、および
1nm以下の二乗平均平方根粗さを有する貴金属被覆銀ナノワイヤーを取得する工程、を含む方法。 - 前記混合物が、室温で、24時間で観察可能な反応を起こさない、請求項6に記載の方法。
- 前記錯化リガンドが、ニトライト(nitrite)、ジエチルアミン、エチレンジアミン、ニトリロ三酢酸、イミノビス(メチレンホスホン酸)、アミノトリス(メチレンホスホン酸)、エチレンジアミン四酢酸(EDTA)、1,3-プロピレンジアミン四酢酸(1,3-PDTA)、トリエチレンテトラミン、トリ(2-アミノエチル)アミン、ジエチレントリアミン五酢酸、1,2-シクロヘキサンジアミノ四酢酸、イミノ二酢酸、メチルイミノ二酢酸、N-(2-アセトアミド)イミノ酢酸、N-(2-カルボキシエチル)イミノ二酢酸、N-(2-カルボキシメチル)イミノジプロピオン酸、ピコリン酸、ジピコリン酸、ヒスチジン、それらの組合せからなる群から選択される、請求項6または請求項7に記載の方法。
- 前記反応溶液が、少なくとも60℃の温度に加熱される、請求項6~8のいずれか一項に記載の方法。
- 前記貴金属源溶液が、貴金属イオン当たり少なくとも2つのリガンド分子を含む、請求項8に記載の方法。
- 前記反応溶液が、キャッピングポリマーを含み、ここで、前記コーティング溶液が、0.0001M~5Mの貴金属イオンを含み、前記反応溶液が、0.01重量%~3.5重量%の銀ナノワイヤーおよび0.01重量%~1.5重量%のキャッピングポリマーを含む、請求項6~10のいずれか一項に記載の方法。
- 0.05重量%~15重量%の貴金属を有する貴金属被覆銀ナノワイヤーを取得する工程をさらに含む、請求項6~11のいずれか一項に記載の方法。
- 前記貴金属被覆銀ナノワイヤーが、平均直径の10パーセント以下の標準偏差で、前記ナノワイヤーの長さに沿ってある直径を有し、少なくとも0.02原子パーセントの貴金属を有する、請求項1~12のいずれか1項に記載の方法。
- 前記貴金属被覆銀ナノワイヤーが少なくとも0.1原子パーセントの貴金属を含む、請求項1~13のいずれか一項に記載の方法。
- 前記貴金属が、金、白金またはそれらの組合せである、請求項1~14のいずれか一項に記載の方法。
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