This work has been performed at the Molecular Foundry, Lawrence Berkeley National Laboratory and supported by the Office of Science, Office of Basic Energy Sciences, Scientific User Facilities Division of the US Department of Energy, under Contract No. DE-AC02&#8211;05CH11231. The financial support of F.M. by a ME-Fulbright fellowship and A.S. by Higher Education Commission of Pakistan are gratefully acknowledged.

注：開始する前に、関連するすべての材料データシート（MSDSを）を確認します。合成およびアプリケーションの手順で使用される化学物質のいくつかは有毒です。すべての適切な安全対策に従って、適切な保護具（白衣、フルレングスのパンツ、閉じたつま先の靴、安全眼鏡、手袋）を使用してください。窒素吸着測定のために液体窒素（絶縁手袋、フェースシールド）を取り扱う際は、すべての極低温個人用保護具を使用してください。 バルクとキャピラリカラム形式で1多孔質ポリマーモノリスの準備<ol><li>特性評価のためのバルクポリマーモノリス<ol><li>重合抑制剤を除去するために、塩基性アルミナのカラムに通し、スチレン、ジビニルベンゼン、メタクリル酸を精製します。シリンジチップに詰めたガラスウール繊維のプラグ付きの25ミリリットル使い捨てのプラスチック製注射器に塩基性アルミナ10gを配置します。カラムを通して単量体の約10ミリリットルを浸透。 </li><li>モノマー（50 mgのスチレン、100mgのジビニルベンゼンおよび50mgメタクリル酸）および1ミリリットルのガラスバイアルの孔形成剤（300 mgのトルエンと300ミリグラムイソオクタン）をロードします。重合開始剤、2,2&#39;-アゾビスイソブチロニトリル（AIBN、モノマーに対して1％）の4ミリグラムを追加します。 </li><li> 10分間の超音波処理によってホモジナイズします。 10分間液体窒素をバブリングすることによって溶存酸素を除去します。パラフィンフィルムでバイアルキャップを密封し、混合物を重合するために6時間、60℃の水浴中に置き。 </li><li>室温まで冷却し、慎重にバイアルを破ります。セルロース抽出シンブルにポリマーモノリスを転送します。ソックスレー抽出チャンバ内に抽出シンブルに入れ、抽出チャンバの少なくとも3倍の体積であるメタノールの量が含まれている丸底フラスコに組み立てます。抽出チャンバーの上部にコンデンサーを組み立てます。メタノールを沸騰させてソックスレー抽出を行います16時間、未反応モノマーおよび孔形成剤の完全な除去を確実にします。 </li><li> 60℃の真空オーブンで一晩乾燥。赤外分光法（FT-IR）をフーリエ変換することによりPCPを取り付けるためのカルボン酸官能基の存在を確認します。窒素吸着ポロシメータによって表面積を測定します。 </li></ol></li><li>モノリシックカラムの作製のためのシリカキャピラリーの機能化<ol><li>ポリイミドコーティングされた100ミクロンのID溶融シリカキャピラリーの2メートルをカット。 0.25〜0.50ミリリットルのガラス製注射器に接続し、アセトンでキャピラリーを洗浄します。水でキャピラリーをすすぐことによりアセトンを除去。 </li><li>キャピラリーの内部シリカコーティングを活性化するために、30分間、0.25μL/分で0.2 M NaOH水溶液を流すシリンジポンプを使用。流出液が中性になるまで水で洗い流してください。 </li><li>流出液のpHをチェックするためにpH試験紙ストリップを使用してください。キャピラリーのシラノール基をプロトン化するために、0.2 M aqueoポンプ30分間、0.25マイクロリットル/分でキャピラリーを通して私たちのHCl溶液。流出液が中性になるまで水で洗い流してください。エタノールですすいでください。 </li><li> 0.25μlの1時間/分で、3-（トリメトキシシリル）プロピルメタクリレート（pH5の酢酸で調節）の20％（w / w）のエタノール溶液をポンプ。このステップでは、シリカキャピラリーは、キャピラリー内表面にポリマーモノリスを取り付けるためにビニル基で官能化されます。 </li><li> 、アセトンですすぎ、窒素気流中で乾燥し、使用前に室温で一晩おきます。長さ20cmの短い断片にキャピラリをカット。 </li></ol></li><li>モノリシックキャピラリカラムの調製<ol><li>ゴム隔壁を1ミリリットルのガラスバイアルにバルクポリマーモノリス（セクション1.1）のためのものと同一の重合混合物を準備します。モノマーに対する開始剤を1％AIBNを追加します。 10分間の超音波処理によってホモジナイズします。 </li><li>非官能基化シリカキャピラリーを結合することによって、窒素で重合混合物をパージ窒素気流へ。 <ol><li>バイアルのゴム隔壁を通して窒素流キャピラリーを挿入し、窒素が液体を介して気泡ように重合混合物にそれを浸します。過剰圧力を回避するために、少し緩いバイアルキャップを残します。 10分間パージします。 </li><li>バイアルのヘッドスペースに重合混合物から窒素流キャピラリーを持ち上げ、しっかりとキャップを閉じます。重合混合物中にセプタムを通して官能キャピラリを挿入します。ヘッドスペース内に注入窒素を介してキャピラリーに発生する圧力の過剰は、官能毛細管を通して重合混合物をポンプ。 </li><li>それが完全に満たされることを確実にするために、毛細管の流出物から重合混合物を数滴を収集し、ゴム隔膜で閉じます。非常に慎重にバイアルからキャピラリを取り、ゴム隔膜でキャピラリーの入口を閉じます。 </li></ol></li><li>ミックスを重合6時間、60℃の水浴中でキャピラリー内に含まれるチャー。室温で冷却し、キャピラリーの両端の数ミリを切りました。 30分間の3μL/ minでHPLCポンプを用いてアセトニトリルでカラムを洗浄することにより未反応モノマーおよび孔形成剤を除去します。キャピラリカラムの背圧を確認してください。 </li></ol></li></ol>鉄benzenetrycarboxylate 2.成長（FeBTC）PCP <ol><li>特性評価のためのバルクポリマーモノリスのFeBTC MOPHの成長<ol><li>乳鉢と乳棒を用いて予め乾燥モノリスを粉砕。 </li><li> 15分間、エタノール中の2mMのFeCl 3·6H 2 O 5ml中モノリス粉末100mgを浸し。ナイロンフィルター（0.22μm）を用いて、真空フィルター、エタノールで粉末を洗浄します。 15分間、エタノール中の2 mMの1,3,5-ベンゼントリカルボン酸（BTC）5ml中モノリス粉末を浸し。ナイロンフィルター（0.22μm）を用いて、真空フィルター、エタノールで粉末を洗浄します。</li><li>必要に応じて、ステップ数2を繰り返します。最終的な有機金属被膜の成長は、適用されたサイクル数によって定義されます。典型的には、10〜30サイクルが行われます。窒素吸着ポロシメータによる新たな細孔が存在することを確認してください。熱重量分析（TGA）によって、追加の金属部位の量を測定します。 </li></ol></li><li>ホスホペプチドの濃縮のためのキャピラリーモノリスカラム上FeBTC MOPHの成長<ol><li>シリンジポンプを使用しました。 2μL/分で15分間、エタノール中の2mMのFeCl 3·6H 2 Oでキャピラリーモノリスをフラッシュします。 2μL/分で15分間、エタノールで洗浄します。 2μL/分で15分間、エタノール中の2 mMのBTCとキャピラリーモノリスをフラッシュします。 2μL/分で15分間、エタノールで洗浄します。 </li><li>必要に応じて、ステップ1を繰り返します。最終的な有機金属被膜の成長を行うサイクルの数によって定義されます。 </li></ol></li></ol> 3.タンパク質消化およびEリン酸化ペプチドのnrichment <ol><li>タンパク消化<ol><li> 1mlの水に無脂乳0.5mlのを溶解し、200μlの画分に分割します。 </li><li>タンパク質消化のためのジスルフィド結合を切断するために、各画分に160μlの1 M重炭酸アンモニウムと50μlの45mMのジチオスレイトールを追加します。 15分間、サーモミキサーで50℃でインキュベートします。 </li><li>溶液を室温まで冷却しながら、ヨードアセトアミドの100mM水溶液を徐々に50μlを添加します。ヨードアセトアミドは、新たなジスルフィド結合の形成を防ぐことができます。 </li><li>室温で15分間、暗所でインキュベートします。脱イオン水1ミリリットルを追加します。 2μgのトリプシンを添加し、14時間、37℃でサーモ中のタンパク質を消化します。 </li><li> 1％トリフルオロ酢酸の10μlの酸性化によって消化を終了し、そして室温で5分間サーモミキサーに入れます。 -20℃で消化したタンパク質を保存します °C。 </li></ol></li><li>キャピラリMOPHカラムを用いてリン酸化ペプチドの濃縮。 <ol><li> 1μL/分の流速で10分間、0.1％トリフルオロ酢酸を含有するアセトニトリルの4：1混合物100μlでカラムを洗浄します。 30分間、2μL/分でカラムに通してタンパク質消化ポンプ。 </li><li> 1μL/分の流速で10分間、0.1％トリフルオロ酢酸を含有するアセトニトリルの混合物1：4で再び非リン酸化ペプチドを洗浄します。 1μL/分の流速で10分間水で洗浄します。 </li><li> 15分間、1μL/分でポンピング250mMのpH7のリン酸緩衝液を用いてリン酸化ペプチドを溶出させます。バイアルに溶離液を収集し、標準的なプロトコル19を用いて、溶液を脱塩します。マトリックス支援レーザー脱離/イオン化飛行時間型質量分析法（MALDI-TOF-MS）のためのマトリックスとして使用するために2 mg / mlの2,5-ジヒドロキシ安息香酸を調製します。 phosphopeを溶出するために、先端に2,5-ジヒドロキシ安息香酸の2μLを描かptidesとMALDIプレート上に直接それらを見つけます。 </li><li> MALDI-TOF-MSによるスポットを分析し、水、次いでメタノールで十分に洗い流すことによって列を再生成します。 </li></ol></li></ol>

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The authors have nothing to disclose.

元のポリマーモノリスは、金属に結合することができるカルボン酸官能基を含んでいます。元の材料に初期金属部位の調整、我々は、微孔性ネットワークを成形する付加的な金属部位の数を取り入れ、PCPコーティング（ 図1A）を増殖することができます。これは、固定化金属イオンアフィニティークロマトグラフィー（IMAC）法などの金属種が関与している抽出または精製手順の?...

多孔性配位高分子（のPCP）は、非晶質または結晶質であってもよい1-3 1、2または3次元に延びる調整エンティティを繰り返し、有機リガンドにより結合された金属中心に基づいて、配位化合物です。近年では、多孔性材料のこのクラスは、それらの高い多孔性、広い化学調整可能性、及びその安定性に広く注目を集めています。のPCPは、ガス貯蔵、ガス分離、および触媒3-6を含むアプリケーションの範囲について検討されており、非常に最近のPCPの最初の分析アプリケーションは、7に記載されています。 そのため、その強化された化学官能性と高気孔率のPCPの精製プロセスおよびクロマトグラフィー分離の改善のための巨大な潜在的な対象のされており、このトピックに関するレポートの数は7-13を公開されています。しかし、のPCPの性能はequivaleで、現在ではありませんそれらの粒子または結晶のそれらの一般的に不規則な形状の形態に起因するこれらの固体の充填床に大きな粒子間の空隙を介して高速拡散する可能性が高い既存のクロマトグラフィー材料とNTレベル。この不規則に分布パッキンが予想より低い性能だけでなく、高いカラム背圧、望ましくないピーク形状形態14,15につながります。 粒子間の空隙を介して高速拡散の問題を解決し、同時に分析アプリケーションのためのPCPの性能を高めるために、マクロ細孔の表面にPCPを含んでいるマクロ多孔性ポリマーモノリス16に基づいて、ハイブリッド材料の開発希望ことが望ましいこと。ポリマーモノリスは、それらパッキンをビーズに最も効率的な代替手段の一つであり、正常にいくつかのCによって商品化されていることができており、その孔を通して対流を維持することができる自己完結型、シングルピースの材料であります<html> ompanies 17,18。多孔質ポリマーモノリスは、通常、モノマーの重合と、典型的には、有機溶媒の二成分混合物であるポロゲンの存在下で架橋剤に基づいています。得られたモノリス材料はmicroglobular構造と高気孔率と流れ透過性を有します。 PCPを含むポリマーモノリスを調製するために、これらの材料を統一するための単純なアプローチは、モノリスの重合混合物のような合成のPCPの直接添加に基づいています。このアプローチは、主にポリマー骨格内に埋め込 ​​まのPCPをもたらし、最終的な材料14,15のさらなる適用のためにアクティブではありません。別の合成アプローチは、明らかに、例えば、結晶中に含まれる気孔の大部分は、ポリマーモノリスのマクロ孔からアクセス可能であるのPCP、または結晶質の金属有機構造体（MOF）の均一な膜を開発するために必要とされます。 tは &quot;&gt;ここで、我々は簡単に自己完結型の単として実装することができるのPCPの取り付けに適した官能基を有するマクロ多孔性ポリマー支持体に基づく有機金属ポリマーハイブリッド材料（MOPH）の調製のための簡単​​なプロトコルを報告しますフロースルーのアプリケーションに最適な特性を有する列形式で-pieceポリマーモノリス。ポリマー合成手順は、単純な室温の溶液系が続きます&#160;モノリス19-20の孔の内面にPCPコーティングを成長させる方法。第1の例として、我々は、マクロ孔質ポリ（スチレン - ジビニルベンゼン - メタクリル酸）モノリス内の鉄（III）benzenetricarboxylate（FeBTC）配位ポリマーフィルムの調製を記載します。この方法は、バルク粉末の調製並びにキャピラリカラムのために効果的であると記載されているプロトコルは、他のPCPに容易に実装可能です。フローthrouのための機能性材料としてMOPHsの電位の例として、GHアプリケーションでは、我々は、Fe（III）の緻密なコーティングは、Fe（III）へのリン酸化の結合親和性を利用する消化されたタンパク質の混合物からリン酸化ペプチドを豊かにする中心含まれている開発FeBTC MOPHを適用しました。開発されたプロトコル21は、3つの主要部分を含む：マクロポーラス有機ポリマーモノリス担体の調製;モノリスの細孔の表面にPCPコーティングの成長;ホスホペプチドの濃縮のためのアプリケーションです。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Polyimide-coated capillaries</td>
			<td>Polymicro Technologies</td>
			<td>TSP100375</td>
			<td>100 &#956;m i.d.</td>
		</tr>
		<tr>
			<td>3-(trimethoxysilyl)propyl methacrylate, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>440159</td>
			<td></td>
		</tr>
		<tr>
			<td>Styrene, 99%</td>
			<td>Sigma-Aldrich</td>
			<td>W323306</td>
			<td>Technical grade</td>
		</tr>
		<tr>
			<td>Divinylbenzene, 80%</td>
			<td>Sigma-Aldrich</td>
			<td>414565</td>
			<td></td>
		</tr>
		<tr>
			<td>Methacrylic acid, 98%</td>
			<td>Mallinckrodt</td>
			<td>MK150659</td>
			<td></td>
		</tr>
		<tr>
			<td>Toluene, &#8805;99.5%</td>
			<td>EMD chemicals</td>
			<td>MTX0735-6</td>
			<td></td>
		</tr>
		<tr>
			<td>Isooctane, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>650439</td>
			<td></td>
		</tr>
		<tr>
			<td>2,2&#39;-azobisisobutyronitrile, 98%</td>
			<td>Sigma-Aldrich</td>
			<td>441090</td>
			<td></td>
		</tr>
		<tr>
			<td>Aluminium oxide (basic alumina)</td>
			<td>Sigma-Aldrich</td>
			<td>199443</td>
			<td></td>
		</tr>
		<tr>
			<td>Iron (III) chloride hexahydrate, 97%</td>
			<td>Sigma-Aldrich</td>
			<td>236489</td>
			<td></td>
		</tr>
		<tr>
			<td>1,3,5-benzenetrycarboxylic acid, 95%</td>
			<td>Sigma-Aldrich</td>
			<td>482749</td>
			<td></td>
		</tr>
		<tr>
			<td>Acetonitrile, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>360457</td>
			<td></td>
		</tr>
		<tr>
			<td>Ammonium bicarbonate, &#8805;99.5%</td>
			<td>Sigma-Aldrich</td>
			<td>9830</td>
			<td></td>
		</tr>
		<tr>
			<td>Trifluoroacetic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>302031</td>
			<td></td>
		</tr>
		<tr>
			<td>Ethanol, &#8805;99.8%</td>
			<td>Sigma-Aldrich</td>
			<td>2854</td>
			<td></td>
		</tr>
		<tr>
			<td>Iodoacetamide, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>I1149</td>
			<td></td>
		</tr>
		<tr>
			<td>Dithiothreitol, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>43819</td>
			<td></td>
		</tr>
		<tr>
			<td>Monobasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71505</td>
			<td></td>
		</tr>
		<tr>
			<td>Dibasic sodium phosphate dihydrate, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>71643</td>
			<td></td>
		</tr>
		<tr>
			<td>Phosphoric acid, &#8805;85%</td>
			<td>Sigma-Aldrich</td>
			<td>438081</td>
			<td></td>
		</tr>
		<tr>
			<td>2,5-dihydroxybenzoic acid, &#8805;99%</td>
			<td>Sigma-Aldrich</td>
			<td>85707</td>
			<td></td>
		</tr>
		<tr>
			<td>Trypsin</td>
			<td>Sigma-Aldrich</td>
			<td>T8003</td>
			<td>Bovine pancreas</td>
		</tr>
		<tr>
			<td>&#946;-casein</td>
			<td>Sigma-Aldrich</td>
			<td>C6905</td>
			<td>Bovine milk</td>
		</tr>
		<tr>
			<td>ZipTip pipette tips</td>
			<td>Merck Millipore</td>
			<td>ZTC18S096</td>
			<td>C18 resin</td>
		</tr>
	</tbody>
</table>

preparation of highly porous coordination polymer coatings on macroporous polymer monoliths for enhanced enrichment of phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

有機ポリマーモノリスの細孔表面上のPCPの成長の概略図を図1に示す。この図では、我々は、カルボキシル官能基に配位し、元のポリマーモノリスの細孔表面上に保持され、初期のFe（III）原 ​​子を例示します。プロトコルを使用して、本明細書中に追加の有機配位子とを記載したFe（III）イオンは、ポリマーモノリス内の多孔性配位ネットワークを成形、表面に添加されてい?...

Watch this Scientific Journal Video about Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides at JoVE.com

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

リン酸化ペプチドの強化充実のためのマクロポーラスポリマーモノリスの高度に多孔性配位高分子コーティングの製造

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

preparation-highly-porous-coordination-polymer-coatings-on

Research

JoVE Journal

Chemistry

10.0K ビュー.  E. O. Lawrence Berkeley National Laboratory. A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

ビデオ: Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

監禁静止と流れるコロイド·ポリマー混合物の共焦点イメージング

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

化学

Fabrication of Large-area Free-standing Ultrathin Polymer Films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

大面積自立超薄ポリマーフィルムの作製

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

ポリマー/フラーレンナノ粒子の光増感を実施ブレンドと光線力学療法

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

Preparation of Macroporous Epitaxial Quartz Films on Silicon by Chemical Solution Deposition

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step process based on the preparation of a sol in a one-pot synthesis which is followed by the deposition of a gel film on Si(100) substrates by evaporation induced self-assembly using the dip-coating technique and ends with a thermal treatment of the material to induce the gel crystallization and the growth of the quartz film. The formation of a silica gel is based on the reaction of a tetraethyl orthosilicate and water, catalyzed by HCl, in ethanol. However, the solution contains two additional components that are essential for preparing mesoporous epitaxial quartz films from these silica gels dip-coated on Si. Alkaline earth ions, like Sr2+ act as glass melting agents that facilitate the crystallization of silica and in combination with cetyl trimethylammonium bromide (CTAB) amphiphilic template form a phase separation responsible of the macroporosity of the films. The good matching between the quartz and silicon cell parameters is also essential in the stabilization of quartz over other SiO2 polymorphs and is at the origin of the epitaxial growth.

A protocol is presented for the preparation of piezoelectric macroporous epitaxial films of quartz on silicon by solution chemistry using dip-coating and thermal treatments in air.

化学溶液法によるシリコン上のマクロポーラスエピタキシャル石英薄膜の作製

This work describes the detailed protocol for preparing piezoelectric macroporous epitaxial quartz films on silicon(100) substrates. This is a three-step ...

Functionalization of Single-walled Carbon Nanotubes with Thermo-reversible Block Copolymers and Characterization by Small-angle Neutron Scattering

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous solution. In a carbon nanotube/PEO105-PPO70-PEO105 (poloxamer 407) aqueous solution, the amphiphilic poloxamer 407 adsorbs onto the carbon nanotube surfaces and self-assembles into continuous layers, driven by intermolecular interactions between constituent molecules. The addition of 5-methylsalicylic acid changes the self-assembled structure from spherical-micellar to a cylindrical morphology. The fabricated poloxamer 407/carbon nanotube hybrid particles exhibit thermo-responsive structural features so that the density and thickness of poloxamer 407 layers are also reversibly controllable by varying temperature. The detailed structural properties of the poloxamer 407/carbon nanotube particles in suspension can be characterized by small-angle neutron scattering experiments and model fit analyses. The distinct curve shapes of the scattering intensities depending on temperature control or addition of aromatic additives are well described by a modified core-shell cylinder model consisting of a carbon nanotube core cylinder, a hydrophobic shell, and a hydrated polymer layer. This method can provide a simple but efficient way for the fabrication and in-situ characterization of carbon nanotube-based nano particles with a structure-tunable encapsulation.

A method for the functionalization of carbon nanotubes with structure-tunable polymeric encapsulation layers and structural characterization using small-angle neutron scattering is presented.

小角中性子散乱による熱可逆性ブロック共重合体と特性を持つ単層カーボンナノチューブの機能化

We demonstrate a protocol for single-walled carbon nanotube functionalization using thermo-sensitive PEO-PPO-PEO triblock copolymers in an aqueous ...

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

サーモ可逆架橋ゴム経由アルダー化学の合成と性質

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

Monitoring the Effects of Illumination on the Structure of Conjugated Polymer Gels Using Neutron Scattering

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and absence of white light exposure. By instituting a controlled temperature ramp, the gelation of these materials can be precisely monitored as they proceed through this structural evolution, which effectively mirrors the conditions experienced during the solution deposition phase of organic electronic device fabrication. Using small angle neutron scattering (SANS) and ultra-small angle neutron scattering (USANS) along with appropriate fitting protocols we quantify the evolution of select structural parameters throughout this process. Thorough analysis indicates that continued light exposure throughout the gelation process significantly alters the structure of the ultimately formed gel. Specifically, the aggregation process of poly(3-hexylthiophene-2,5-diyl) (P3HT) nano-scale aggregates is negatively affected by the presence of illumination, ultimately resulting in the retardation of growth in conjugated polymer microstructures and the formation of smaller scale macro-aggregate clusters.

A protocol for the analysis of gels formed from the optoelectronic conjugated polymer poly(3-hexylthiophene-2,5-diyl) (P3HT) using small and ultra-small angle neutron scattering in both the presence and absence of illumination is presented.

中性子散乱法を用いた共役高分子ゲルの構造に対する光照射効果のモニタリング

We demonstrate a protocol to effectively monitor the gelation process of a high concentration solution of conjugated polymer both in the presence and ...

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

マイクロ流体ドライ回転と再生絹フィブロイン繊維の特性

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

Electrochemical Impedance Spectroscopy as a Tool for Electrochemical Rate Constant Estimation

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). In the case of fast reversible electrochemical processes, current is predominantly affected by the rate of diffusion, which is the slowest and limiting stage. EIS is a powerful technique that allows separate analysis of stages of charge transfer that have different AC frequency response. The capability of the method was used to extract the value of charge transfer resistance, which characterizes the rate of charge exchange on the electrode-solution interface. The application of this technique is broad, from biochemistry up to organic electronics. In this work, we are presenting the method of analysis of organic compounds for optoelectronic applications.

Electrochemical impedance spectroscopy (EIS) of species that undergo reversible oxidation or reduction in solution was used for determination of rate constants of oxidation or reduction.

電気化学インピー ダンス分光電気化学定数推定法のためのツールとして

Electrochemical impedance spectroscopy (EIS) was used for advanced characterization of organic electroactive compounds along with cyclic voltammetry (CV). ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

時間分解光物性評価のトリプレット収穫有機化合物無酸素環境使用、iCCD カメラ

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...