The authors have no acknowledgements.

逐次付加を介してCMP薄膜の合成1。 <ol><li>マイカ上に金の自己組織化単分子膜（SAM）機能化。 <ol><li>エタノール中の11-チオアセチルウンデカン酸-プロパルギルアミド14の1 mM溶液（SAM-液）を準備します。溶液が透明になるまで超音波浴を用いて混ぜます。アルミ箔を用いた光からボトルを保護します。 </li><li>アルゴン下、金雲母のウエーハを得ます。貯蔵容器からの撤退後18時間SAM-溶液に直接マイカウェハを浸します。 </li><li>窒素気流下エタノールとドライですすぎ、SAM-溶液から準備金雲母ウエハを取ります。その後、光から不活性ガス下で保護された基板を格納します。 </li></ol></li><li>前駆体溶液。 <ol><li> 18.64 mgの銅触媒（テトラキス（アセトニトリル）銅（I）ヘキサフルオロリン酸）、20.83ミリグラムのテトラフェニルメタン（TPM）-alkyne及び24.22ミリグラムTPM - アジドを計量し、独立したシュレンクフラスコ中に各コンポーネントを記入してください。TPM-アルキンとTPM-アジ化については、図1を参照してください 、合成は、 文献 15に記載されています。避難し、不活性ガス（N 2またはアルゴン）で3回補充します。 </li><li>各シュレンクフラスコに25ミリリットルの水を含まないテトラヒドロフラン（THF）を追加します。アルミ箔を用いた光からTPMアジドとTPM-アルキンとフラスコを保護します。 </li></ol></li><li> CMPの製造のための装置を準備します。 注：合成装置は、 図2に示されています。 <ol><li> 250ミリリットル1口丸底フラスコを使用してください。 130ミリリットルのTHFに記入してください。アルキンでコーティングされた準備した基板を入れ、サンプルコンパートメントにSAMを終了しました。基板が直立されるように、試料ホルダーを使用してください。 </li><li>還流冷却器の上部に接合を介しシュレンクラインに装置を接続します。 </li><li> 3回避難し、不活性ガスで換気します。 </li></ol></li><li>不活性条件下順次追加。 <ol><li> 90℃に加熱器を設定し、THFは再ですまで待ち​​ますフラックス。 </li><li>サンプルコンパートメントの底部に排出口の上にサンプルコンパートメントからTHFをしてみましょう。コンセントを閉じます。 </li><li>隔壁を有するスクリューキャップを経由してサンプルコンパートメントに準備されたTPM - アジド溶液1mlとCu（I）触媒溶液0.5mlを与えます。反応装置へのシュレンクフラスコからソリューションを順次転送するために中空の針と注射器を使用してください。注意：シーケンスは、反応に影響を及ぼさありません。 </li><li>約30分待ちます。 </li><li>サンプルコンパートメントの底部に排出口の上に反応溶液をしてみましょう。口を閉じて、サンプルを洗浄するための凝縮THFを収集します。約30分待ちます。 </li><li>サンプルコンパートメントの底部に排出口の上にリンス液をしましょう​​。コンセントを閉じます。 </li><li>隔壁を有するスクリューキャップを経由してサンプルコンパートメントに準備されたTPM-アルキン溶液1mlとCu（I）触媒溶液0.5mlを与えます。中空で注射器を使用します針は、反応装置へのシュレンクフラスコからの溶液を順次転送します。注意：シーケンスは、反応に影響を及ぼさありません。 </li><li>約30分待ちます。 </li><li>サンプルコンパートメントの底部に排出口の上に反応溶液をしてみましょう。口を閉じて、サンプルを洗浄するための凝縮THFを収集します。約30分待ちます。 </li><li>反復は、層の所望の量に到達するまで1.4.9 1.4.3するステップ。注：1つの層が1nm程度の厚さです。 </li><li> 、CMP被覆マイカ基板を取り出し、THF、エタノールでそれを洗浄し、窒素気流下でそれを乾燥させます。 </li></ol></li></ol> CMPナノ薄膜の2転送<ol><li>ポリ（メチルメタクリレート）（PMMA）の溶液。 <ol><li>酢酸エチル中4％（重量）、PMMA（M 996キロダルトン）の溶液を調製します。溶液が透明になるまで超音波浴を用いて、PMMAを溶解します。 </li></ol></li><li> PMMA溶液のスピンコーティング。 <ol><li> RAにスピンコーターを設定0〜4000 RPMからのMP時間10秒、40秒の時間を保持し、4000から0 RPMまでの時間10秒をランプアップします。 </li><li>スピンコーターのCMPコーティングされたマイカ基板を配置し、それが完全に覆われるまで、ウェハ上にPMMA液を入れました。スピンコーターを開始します。 </li><li>スピンコーティングが完了した後、90℃の加熱板上で5分間サンプルを置きます。 </li><li>コー​​ティングされたマイカ基板の各エッジから1ミリメートルをカット。エッジをカットするはさみを使用してください。 </li></ol></li><li> PMMAの譲渡は、CMPナノ膜をコーティングしました。 <ol><li> O KI / H 2 / I 2の溶液を調製し（1：4：40メートル/ m / m）のとKI / H 2 Oの（1:10 m / m）の 。 </li><li>結晶皿150ミリリットルのI 2 / KI H 2 O溶液を記入し、結晶皿100ml中のKI / H 2 O溶液を記入してください。 I 2 / KI / H 2 O溶液の上に、この溶液に接触してマイカで、マイカ基板上にコーティングされたPMMAのCMP金を入れてください。それは沈まないように注意してください。少なくとも5分待ってください。 </li><li>液に接触したマイカで、KI / H 2 O溶液の上に、I 2 / KI / H 2 O溶液から、PMMAコーティングされたCMP金雲母基板を置きます。それは沈まないように注意してください。少なくとも5分待ってください。 </li><li>結晶皿250mlの蒸留水を記入してください。雲母からPMMA / CMP /金膜を取り除きます。蒸留水に、一方の端から始めて、少し基板を浸漬することによってこれを行います。マイカは水を指しているように、基板を保持します。注：手順は、 図3に示されています。 </li><li>ディップコートシリコンウェハ上にPMMA / CMP /ゴールド。それは水泳PMMA / CMP /金膜の端に触れるまでウェハでゆっくりとPMMA / CMP /金に接近することによってこれを行います。 SiウエハをPMMA / CMP /金膜に接していると、ゆっくりとシリコンウエハを引き出します。 </li><li>シリコンウエハからPMMA / CMP /金膜を取り除きます。わずか1編から始まり、基板を浸漬することによってこれを行いますI 2 / KI / H 2 O溶液中のGe、。 15分待ってください。 </li><li>金を完全にエッチングした後、シリコンウェハを介して水にPMMA / CMP膜を転送します。 15分待ってください。 </li><li>水でメンブレンを洗浄するための手順を繰り返し2.3.7 3回。 </li><li>ステップ2.3.5で説明した方法を経由して、所望の基材、 例えば、顕微鏡スライドまたは金コーティングされたシリコンウエハに洗浄し、PMMA / CMP膜を転送します。少なくとも2時間、空気中のPMMA / CMP基板を乾燥させてください。 </li></ol></li><li> PMMAの溶解。 <ol><li>アセトンでPMMA / CMP基板を置きます。 30分待ってください。基板を取り出し、アセトンでそれをすすいでください。 </li><li>繰り返しステップ2.4​​.1 3回。 </li><li>少なくとも2時間のCMP基板を乾燥させてください。 </li></ol></li></ol>

<ol>
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A., W&#246;ll, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=MOF+thin+films:+existing+and+future+applications.">MOF thin films: existing and future applications.</a> Chemical Society Reviews. 40 (2), 1081-1106 (2011).</li><li>Liu, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deposition+of+Metal-Organic+Frameworks+by+Liquid-Phase+Epitaxy:+The+Influence+of+Substrate+Functional+Group+Density+on+Film+Orientation.">Deposition of Metal-Organic Frameworks by Liquid-Phase Epitaxy: The Influence of Substrate Functional Group Density on Film Orientation.</a> Materials. 5 (9), 1581-1592 (2012).</li><li>Such, G. K., Quinn, J. F., Quinn, A., Tjipto, E., Caruso, F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Assembly+of+Ultrathin+Polymer+Multilayer+Films+by+Click+Chemistry.">Assembly of Ultrathin Polymer Multilayer Films by Click Chemistry.</a> Journal of the American Chemical Society. 128 (29), 9318-9319 (2006).</li><li>Ai, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Carbon+Nanomembranes+(CNMs)+Supported+by+Polymer:+Mechanics+and+Gas+Permeation.">Carbon Nanomembranes (CNMs) Supported by Polymer: Mechanics and Gas Permeation.</a> Advanced Materials. 26 (21), 3421-3426 (2014).</li><li>Jiang, J. -. X., Cooper, A. 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J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Nanoporous+organic+polymer+networks.">Nanoporous organic polymer networks.</a> Progress in Polymer Science. 37 (4), 530-563 (2012).</li><li>Muller, T., Br&#228;se, S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Click+Chemistry+Finds+Its+Way+into+Covalent+Porous+Organic+Materials.">Click Chemistry Finds Its Way into Covalent Porous Organic Materials.</a> Angewandte Chemie International Edition. 50 (50), 11844-11845 (2011).</li><li>Tsotsalas, M., Addicoat, M. 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K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+modular+approach+for+the+construction+and+modification+of+glyco-SAMs+utilizing+1,3-dipolar+cycloaddition.">A modular approach for the construction and modification of glyco-SAMs utilizing 1,3-dipolar cycloaddition.</a> Organic &amp; Biomolecular Chemistry. 6 (12), 2118-2132 (2008).</li><li>Plietzsch, O., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Four-fold+click+reactions:+Generation+of+tetrahedral+methane-+and+adamantane-based+building+blocks+for+higher-order+molecular+assemblies.">Four-fold click reactions: Generation of tetrahedral methane- and adamantane-based building blocks for higher-order molecular assemblies.</a> Organic &amp; Biomolecular Chemistry. 7, (2009).</li><li>Greenler, R. 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The authors have nothing to disclose.

CMP-フィルムの合成用触媒の溶液を新鮮にする必要があります。壊れた触媒（ すなわち、酸化された）を、溶液の青色着色によって示されます。新鮮な溶液は無色です。 重要な点は、スピンコートPMMA後マイカ基板の端部を切断することです。また、基板の欠陥をカットする必要があり、 すなわち、各スポットは、PMMAが見つからないため、金層の、マイカ?...

The preparation of ultra-thin polymer membranes is of high interest for applications in gas separation and nanofiltration. Challenges in the synthesis are represented by (a) the control of the membrane thickness and the homogeneity and (b) transfer of such fragile membranes. To overcome challenge (a), molecular layer-by-layer synthesis1 has shown great promise in controlling the thickness and homogeneity of thin films grown at the solid-liquid interface.2,3 Controlling the number of layers linearly controls the film thickness. The l-b-l method has been successfully used to fabricate surface mounted metal organic frameworks (SURMOFs),4-7 also the synthesis of thin polymer films via l-b-l reaction of polymer chains was demonstrated.8 The challenge (b) concerns the handling of these ultra-thin membranes. To avoid rupture or wrinkling of the nanomembranes sacrificial supports of coatings have shown great promise. 9
Here we will present a detailed protocol for synthesis of conjugated microporous polymer (CMP)10-13 thin films through sequential addition of the molecular building blocks, with desired thickness and composition. The preparation of free-standing CMP nanomembranes is achieved by using a sacrificial support. To handle and transfer the CMP nanomembranes to other supports we will describe a simple protocol to protect the membranes with sacrificial coatings and their upfloating to the liquid air interface and subsequent transfer using dip-coating.

<table>
	<tbody>
		<tr>
			<td>Acetone</td>
			<td>VWR BDH Prolabo</td>
			<td>20066.330</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Potassium iodide</td>
			<td>VWR BDH Prolabo</td>
			<td>26846.292</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Ethyl acetate</td>
			<td>VWR BDH Prolabo</td>
			<td>23882.321</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Tetrahydrofurane (THF)</td>
			<td>VWR BDH Prolabo</td>
			<td>28559.320</td>
			<td>HiPerSolv CHROMANORM</td>
		</tr>
		<tr>
			<td>THF waterfree</td>
			<td>Merck Millipore</td>
			<td>1.08107.1001</td>
			<td>SeccoSolv</td>
		</tr>
		<tr>
			<td>Iodine</td>
			<td>Sigma-Aldrich</td>
			<td>20,777-2</td>
			<td></td>
		</tr>
		<tr>
			<td>Tetrakis(acetonitrile)copper(I)hexafluoro-phosphate</td>
			<td>Sigma-Aldrich</td>
			<td>346276-5G</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly(methyl methacrylate) 996 kDa (PMMA)</td>
			<td>Sigma-Aldrich</td>
			<td>182265-25G</td>
			<td></td>
		</tr>
		<tr>
			<td>1.1.1.1 Methanetetrayltetrakis(4-azidobenzene) (TPM-azide)</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to9</td>
		</tr>
		<tr>
			<td>1.1.1.1 Methanetetrayltetrakis(4-ethinylenebenzene) (TPM-alkyne)</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to9</td>
		</tr>
		<tr>
			<td>11-thioacetyl-undecaneacid propargylamide</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to8</td>
		</tr>
		<tr>
			<td>gold/titan coated silicium-wafer</td>
			<td>Georg Albert PVD, 76857 Silz, Germany</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>gold coated mica</td>
			<td>Georg Albert PVD, 76857 Silz, Germany</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

layer-by-layer synthesis and transfer of freestanding conjugated microporous polymer nanomembranes

CMPのような大きな表面積材料は、それらのその優れた熱的および化学的安定性と組み合わせた官能基を組み込むことで高い可変性​​、及び低濃度に、最近関心を集めています。例えば、スピンコーティングなどの通常適用技術が利用できないので、それらの不溶性の性質は、それらの処理に問題を引き起こします。特にCMP薄膜としての処理が望まれる膜の用途のために、処理上の問題は、それらの商業的用途を妨げてきました。 ここでは、分子層ごと（LBL）合成により官能化基材上に、CMP薄膜の界面合成が記載されています。このプロセスは、所望の厚さおよび組成、さらには所望の組成勾配を有するフィルムの製造を可能にします。 犠牲支持体の使用は、後に、支持体の溶解によって自立膜の製造を可能にします合成。このような超薄型自立膜を処理するには、犠牲コーティングと保護は、ナノ薄膜の破裂を避けるために、大きな期待を示しました。所望の基板にナノ薄膜を転送するには、コーティングされた膜は、気液界面でのupfloatedした後、ディップコーティングを介して転送されます。

膜は、赤外反射吸収分光法（IRRAS）によって特徴付けられる。16 図4は、金のウエハに転写CMP-膜からIRRA-スペクトルを示します。芳香族骨格の振動からの典型的なバンドは1605センチメートル-1、1515センチメートル-1と1412センチメートル-1です。未反応のアルキン及びアジド基が2,125 -1および1,227 -1で特徴的なバンドによって観察する?...

Watch this Scientific Journal Video about Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes at JoVE.com

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

層ごとの合成と自立共役高分子ナノ薄膜マイクロポーラスの譲渡

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

layer-layer-synthesis-transfer-freestanding-conjugated-microporous

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Chemistry

9.3K ビュー.  Karlsruhe Institute of Technology. In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

ビデオ: Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

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 ...

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.

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 ...

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 ...

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 ...

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 ...

Raman and IR Spectroelectrochemical Methods as Tools to Analyze Conjugated Organic Compounds

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule on the vibrational level of energy. Raman and IR spectroelectrochemistry can be used for advanced characterization of the structural changes in the organic electroactive compounds. Here, the step-by-step analysis by means of Raman and IR spectroelectrochemistry is shown. Raman and IR spectroelectrochemical techniques provide complementary information about structural changes occurring during an electrochemical process, i.e. allows for the investigation of redox processes and their products. The examples of IR and Raman spectroelectrochemical analysis are presented, in which the products of the redox reactions, both in solution and solid state, are identified.

A protocol of step-by-step Raman and IR spectroelectrochemical analysis is presented.

ラマン散乱とツールとしての IR 分光電気化学法共役有機化合物を分析するには

In the presented work, two spectroelectrochemical techniques are discussed as tools for the analysis of the structural changes occurring in the molecule ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.