契約DE-AC52-07NA27344下ローレンス·リバモア国立研究所によって米国エネルギー省の後援で行わこの作品。

1.溶液の調製<ol><li>注射器と0.20μmのシリンジフィルターを用いて、乳酸エチルの60グラムをフィルタリングします。乳酸エチルにポリビニルホルマールの0.3グラムを追加します。 4時間50℃のオーブン中にソリューションを配置します。ポリマーが完全に溶解したかどうかを確認するために静かにバイアルを振ります。 <ol><li>溶液が濁っているか、まだ光の不均一性を示している場合は、別の2時間オーブンにバイアルを返します。このレシピは、典型的には、膜厚30nm程度のために使用される0.5重量％のポリマー溶液のためのものです。より高いポリマー重量含量を有する溶液は、厚い膜のために使用することができます。 </li></ol></li><li> 20ミリリットルのメスフラスコにPDAC試薬を1.0g秤量し、脱イオン（DI）水で測定線にフラスコを充填することにより、PDACの溶液を調製します。貯蔵容器に転送する前に、溶液を穏やかに旋回。 </li></ol> 2.基板の準備<ol><li>注意。濃硫酸60mlのを注ぎます清潔な250mlビーカーに酸。ゆっくりと30％過酸化水素水20 mLを加え。補助金発煙、その後、溶液を穏やかに旋回されるまで待ちます。溶液およびビーカーは非常に高温になり、混合物は腐食性です。 </li><li>ホットプレート上に150ミリメートルペトリ皿を置き、皿に酸を注ぎます。 100℃のホットプレートを設定します。 <ol><li>研磨面を上にして酸に4 &#39;シリコンウエハを配置します。ゆっくりと全面が濡れていることを確認するためにピンセットで中央にウエハを押し下げます。 30分間酸のウェハのままにしておきます。 </li></ol></li><li>ピンセットで酸からウエハを取り外し、噴出ボトルからDI水で十分にウエハの表裏をすすぎます。水は、通常のパターンでシートをオフする必要があります。クリーンベンチ内のウエハを乾燥させます。 </li><li> DI水で最初に使い捨ての3ミリリットル注射器と0.2μmのフィルターを洗浄し、その後、PDAC溶液でフィルターを取り付け、シリンジに液体を描くことによって、およびnは、フィルタを通して液体を押し出します。 </li><li>スピンコーターで洗浄ウェーハをマウントします。シリンジにPDAC液の1.0〜1.2ミリリットルを描き、ウェハの中央にフィルタかかわらず、それを分配します。 15秒間4,000rpmでスピンし、次に（50℃に予熱）ホットプレートにウェハを転送し、それが30秒放置します。 </li><li> DI水で乾燥したPDAC層を洗い流し、クリーンベンチ内でウェハを乾燥させて。 </li></ol> 3.フィルムの作製<ol><li>スピンコーター上にドライPDAC処理されたウェハを置きます。 </li><li>使い捨ての3ミリリットル注射器と2.4の下で手順を使用して、乳酸エチル溶液）で0.45μmのフィルターを洗浄します。 </li><li>預金を200 rpmで10秒間ウェハとスピンの途中で注射器を用いてフィルタを通る乳酸エチル溶液2.5ミリリットル、1700 RPM（所望の膜厚に依存する）で3秒間。ウエハ上に均一な液膜があるはずです。 </li><li>スピンコーターでフィルム乾燥させてそれは（一般的に10〜15分）視覚的に乾燥するまで、10分間（50℃に予熱）ホットプレートの上に置きます。 </li><li> 、リフトオフのために典型的には2センチ×2センチメートルを小さく正方形に映画をDICEが、使用フィルムホルダ（3.5.1-3.5.2）のサイズに応じて、大きくすることができます。あるいは、ウェハサイズのフィルム（3.5.3）を剥離するための2つのスクライブを行います。 注：標準のフィルムホルダーは真ん中に直径13mmの円形の開口部で、19のx 19ミリメートルです。ウェーハサイズのフィルムの場合、ウエハ1より&quot;小さい直径を有するワイヤーフープ（円形に形成され、例えば 、ステンレス鋼線材）を使用します。フィルムは、通常、リフトオフやうねり間に水を吸収するため、円形の開口部が選択されます。フィルムホルダ上で乾燥したように、水を除去し、膜が収縮します。円形の開口部は、応力が均一に分布することができます。 <ol><li>カッティングテンプレート上のウエハを配置します。ストレート電子メールを防ぐために、すべてのエッジがウエハよりも高くされている正方形のテンプレートを使用しますDGEは、ウェハに触れるからスクライブ時に刃を案内するために使用しました。ダイシング時のストレートエッジの配置を導くために2cmの間隔でエッジをマークします。それを整列するために、2つのエッジに対するウェハを押してください。 </li><li> 2つのアライメントマークに沿ってストレートエッジを置き、フィルムをスクライブするストレートエッジに沿って緩やかにカミソリの刃を描きます。フィルムをマークするのに十分な圧力をかけたが、あまりないウェハ自体をマークし、粒子を生成します。より厚い膜では、切断線がはっきり見えるようになります。 </li><li>ウェハからの一枚でフィルムをリフトオフするには、カミソリの刃を備えたウェーハエッジをスクライブ。ウェハ上の2つのフラットの間、ラックアンドピニオン上にウエハをクランプするために十分な幅のストリップをスクライブ。 </li></ol></li><li> DI水で190×100mmの培養皿を埋めます。チルトステージに取り付けられたラックアンドピニオンに大型フラットによってウエハをクランプし、ゆっくりと脱イオン水の中にそれを下げます。フィルムは水線でのウエハから分離​​する必要があります。 <ol><li> WAFを下げ続けますむしろ水線の下リフトオフインターフェイスを押すよりも、ウエハから分離​​するために、フィルムに十分な時間を与える速度でえー。四角の最初の行は、ウエハから離脱しており、表面に浮いている場合には、ウェハの低下を一時停止します。ウェーハサイズのフィルムの場合、フィルムが完全に外れるまで、ウエハを浸漬続けます。 </li><li>水の中にフィルムホルダのヘッドを浸し、フィルムの下に移動します。フィルム端部のいずれかのフープのハンドル端をラインアップし、フィルムでフープをタッチします。成功した場合、フィルムがフープに固執します。 <ol><li>ウェーハサイズのフィルムの場合は、ちょうどセンチメートル離れて端から、スクライブ部の下にワイヤーフープを配置します。フープは、フィルムがフープの周りにラップし、自身に折り返すことができるように、フィルムのエッジとフープ縁との間の一定の距離を保ち、キャプチャを開始する前に、フィルムの下に中央に配置されていることを確認します。 </li></ol></li><li>で水からゆっくりとフープを撤回35°の角度。非常にゆっくりと水からフィルムを持ち上げます。 注：フィルムの約半分が（水面に、すなわち 、通常の）ほぼ90°の水から引き出された後、20nm未満の厚さのフィルムの場合、ホルダーを介してフィルムを引っ張って避けるように角度を増加させます。リフトアウト角度を変更する場合は、フープを介してフィルムを引っ張って避けるために、そのように、ゆっくりと行います。 </li><li>フープが完全に後退されると、乾燥する側に配置します。ダウンフープを入れる前に、フープの底部が液滴の自由であることを確認し、フープと表面との間に液体シールを作成しないように（例えば、ウェーハトレイとして）曲面を使用します。 </li><li>より多くのスクライブ正方形がウエハ上に残っている場合は、水の中にウェーハを下げ続け、手順を繰り返し3.6.1-3.6.4上記残りの正方形のために。 </li><li>フィルムは、O / Nを乾燥させます。 </li></ol></li></ol>

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著者らは、開示することは何もありません。

PDACの基板処理は、任意のサイズの基板が容易にそれらが負（ 例えば 、シリコンやガラス）に帯電していることを条件とする処理することができることを意味、自己制限静電相互作用に基づいています。1-2 13センチまでの非常に大きい薄膜を示す（ 図直径で）唯一の変更は、使用する試薬の量であることと、このプロトコルを使用して製造。最終的な達成可?...

自立ポリマー薄膜は、5-8センサー、1-3 MEMS、触媒又は濾過、4および組織工学などの様々な用途に使用され、これらはまた、閉じ込め下のポリマーの挙動を探索する基礎的な研究のために使用されています。9- 13自立膜は、シリコンウエハ、ガラススライドとは対照的に、このような環状リングまたはフープのような非連続的な基板上に支持されているものです。この作業は、大面積のフィルムまたは高スループット生産のために適している超薄自立ポリマーフィルムのための単純な、反復可能な製造手順を記載しています。これは、ポリ（ビニルホルマール）、ポリスチレン、ポリ（メチルメタクリレート）などの異なるポリマーの様々な互換性があります。これは、13 cmの直径と同じ大きさ、または10 nmと薄い自立膜を製造するために使用することができます。 1）D：自立ポリマーの製造は、3つの基本的なステップで構成されていこのようなウエハやスライド、2） 放出またはリフトオフフィルムの基板から、および支持体上に得られたフィルムの3）、キャプチャなどの伝統的な基板上にポリマーフィルムのeposition。本稿では、さまざまなリリース方法に関する以前の研究で報告された手順を詳しく説明します。14 堆積は、スピンコーティング、蒸着、またはディップコーティングのような塩基性ポリマー薄膜技術の任意の数によって達成することができます。この研究では、標準的なスピンコーティング技術を利用します。 技術&quot;をオフフロートリフト」は、基板から超薄膜を解放するための最も一般的な方法である。この手法では15、膜と基板は、適切な溶媒浴に浸漬されています。溶剤は、フィルムを解放し、それはお風呂のトップにフロートすることができ、フィルムを膨潤し、自発的な剥離を誘発します。最小膜厚できます16：腫れ誘起歪エネルギーで界面剥離エネルギーのバランスをとることによって決定されるにオフフロートリフトを使用してリリースされます<img alt="式（1）" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> （1） Lは膜厚であり、νfはフィルムのポアソン比である場合、Eは、フィルムのヤング率であり、ξは、フィルムの膨潤比であり、γは、剥離の界面エネルギーです。式（1）によって課される制限を回避する一般的な方法は、フィルムと堆積基板との間の犠牲中間層を堆積させることである。17-20この層間溶媒浴に溶解すると、フィルムが解放され、支持体上に捕捉することができ。関連する方法は、犠牲層PR上にフィルムの機械的剥離を使用し、犠牲上層方法であります解散にIOR。21 犠牲材料の使用は、いくつかの責任者の欠点を有します。まず、余分なプロセス材料及び工程の追加は、最適なフィルムの製造条件及び犠牲材料の処理条件との間の妥協を必要とするかもしれません。次に、犠牲材料は、最終的な自立フィルムの機械的特性や純度に影響を与えずに入金することは困難です。第三に、犠牲材料を堆積するためのプロセスを最適化し、全体的な自立膜の製造における動作としての品質を監視する必要があります。14 本研究では、超薄膜のために使用される技術にオフフロートリフトを可能にする、界面剥離エネルギーを低下させる表面改質技術が記載されています。堆積基板は、ポリカチオンpolydiallyldiammoniumクロライド（PDAC）の自己限定、自己最適化に近い単層を組み立てることにより修飾されます。せいでポリカチオンと基板との間の結合の強さは、この表面改質は、その後の処理工程にロバストです。自己制限および近単層形成の自己最適化の性質は実質的にゼロの最適化が必要であり、大面積に容易に拡張可能です。 除去した後、フィルムは、それがフープ状の支持体上に捕捉された溶剤槽の上部に浮かびます。現存する文献に多くの注意を与えていないが、本研究において我々は、引裂きまたは他の方法でフィルムを損傷する可能性を低減する支持体上に大面積の薄膜を捕捉するための技術を説明します。

<table border="0" cellpadding="0" cellspacing="0">
	<tbody>
		<tr>
			<td>Vinylec E</td>
			<td>SPI</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>ethyl lactate, &#62;98%, FCC, FG,</td>
			<td>Sigma-Aldrich</td>
			<td>W244007-1KG-K</td>
			<td></td>
		</tr>
		<tr>
			<td>4&#34; silicon wafers &#60;100&#62;, Single side polished</td>
			<td>International Wafer Service</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>sulfuric acid, 98%, ACS reagent grade</td>
			<td>Sigma-Aldrich</td>
			<td>320501-6X500ML</td>
			<td></td>
		</tr>
		<tr>
			<td>hydrogen peroxide, 30%, semiconductor grade</td>
			<td>Sigma-Aldrich</td>
			<td>316989-3.7L</td>
			<td></td>
		</tr>
		<tr>
			<td>isopropanol, ACS grade, 4 L</td>
			<td>Fisher Scientific</td>
			<td>A464-4</td>
			<td></td>
		</tr>
		<tr>
			<td>dichloromethane, ACS grade</td>
			<td>Alfa-Aesar</td>
			<td>22917</td>
			<td></td>
		</tr>
		<tr>
			<td>deionized water , distilled</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>PDAC reagent (Sigma-Aldrich 409014)</td>
			<td>Sigma-Aldrich</td>
			<td>409014</td>
			<td></td>
		</tr>
		<tr>
			<td>Spin Coater</td>
			<td>Laurell Technologies&#160;</td>
			<td>WS-650-23</td>
			<td></td>
		</tr>
		<tr>
			<td>Barnstead/Thermolyne Super Nuova explosion-proof hot plate&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>explosion-proof forced air oven</td>
			<td>VWR&#160;</td>
			<td>1330 FMS&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>balance with a range of 1 mg to 1020 g</td>
			<td>Mettler Toledo</td>
			<td>MS1003S</td>
			<td></td>
		</tr>
		<tr>
			<td>reflectance spectrometer</td>
			<td>Filmetrics</td>
			<td>F20-UV</td>
			<td></td>
		</tr>
		<tr>
			<td>manipulator consisting of a Klinger tilt stage, a Brinkman rack-and-pinion and a lab jack&#160;</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Cutting tool/template, LLNL-built, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>straight edge, LLNL, no drawings</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Tent hoop, LLNL</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>culture dish 190 mm x 100 mm, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>20 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>250 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>1000 ml beaker, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>60 ml glass vial with plastic stopper&#160;</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>petri dish, 150 mm diameter x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>600 ml beaker x2, Pyrex</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>tweezers, stainless steel</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>cutting blade</td>
			<td>Exacto</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>clean room wipes</td>
			<td>Contec&#160;</td>
			<td>PNHS-99</td>
			<td></td>
		</tr>
		<tr>
			<td>polyester knit 9/91 IPA/DI water wipes</td>
			<td>Contec&#160;</td>
			<td>Prosat&#160;</td>
			<td></td>
		</tr>
		<tr>
			<td>Fluoroware wafer trays</td>
			<td>Ted Pella</td>
			<td>1395-40</td>
			<td></td>
		</tr>
		<tr>
			<td>Nylon Micro fiber (camel hair)</td>
			<td></td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>Disposable BD 3-mL plastic syringe</td>
			<td>VWR</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.2 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>0.45 um&#160; Luer-lock PTFE filters</td>
			<td>Acrodisc&#160;</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

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.

図1は、大面積にわたって自立薄いポリマーフィルムの一例を示しています。この55nmの厚さのポリビニルホルマールフィルムはここに記載の手順を用いて製造した13-cmの直径のスチールフープに取り付けられています。剥離フィルムの引き裂きにつながる欠陥を導入することなく、大面積にわたって生じます。このように、ポリビニルホルマールの本質的な強さがあっても非常に...

Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

Fabrication of Large-area Free-standing Ultrathin Polymer Films

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 ...

fabrication-of-large-area-free-standing-ultrathin-polymer-films

Research

JoVE Journal

Chemistry

15.1K ビュー.  Lawrence Livermore National Laboratory. 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.

ビデオ: Fabrication of Large-area Free-standing Ultrathin Polymer Films

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and lignin. Layer-by-layer (LbL) assembly process which relies on the assembly of oppositely charged molecules from aqueous solutions was used to build a freestanding composite film of isolated wood polymers of lignin and oxidized nanofibril cellulose (NFC). To facilitate the assembly of these negatively charged polymers, a positively charged polyelectrolyte, poly(diallyldimethylammomium chloride) (PDDA), was used as a linking layer to create this simplified model cell wall. The layered adsorption process was studied quantitatively using quartz crystal microbalance with dissipation monitoring (QCM-D) and ellipsometry. The results showed that layer mass/thickness per adsorbed layer increased as a function of total number of layers. The surface coverage of the adsorbed layers was studied with atomic force microscopy (AFM). Complete coverage of the surface with lignin in all the deposition cycles was found for the system, however, surface coverage by NFC increased with the number of layers. The adsorption process was carried out for 250 cycles (500 bilayers) on a cellulose acetate (CA) substrate. Transparent free-standing LBL assembled nanocomposite films were obtained when the CA substrate was later dissolved in acetone. Scanning electron microscopy (SEM) of the fractured cross-sections showed a lamellar structure, and the thickness per adsorption cycle (PDDA-Lignin-PDDA-NC) was estimated to be 17 nm for two different lignin types used in the study. The data indicates a film with highly controlled architecture where nanocellulose and lignin are spatially deposited on the nanoscale (a polymer-polymer nanocomposites), similar to what is observed in the native cell wall.

The objective of this research was to form synthetic plant cell wall tissue using layer-by-layer assembly of nanocellulose fibrils and isolated lignin assembled from dilute aqueous suspensions.&#160; Surface measurement techniques of quartz crystal microbalance and atomic force microscopy were used to monitor the formation of the polymer-polymer nanocomposite material.

Nanocellulose、リグニンから製造自立フィルム、合成ポリカチオン：Biomimickingウッドに向けて

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and ...

化学

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 ...

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 ...

Cooling Rate Dependent Ellipsometry Measurements to Determine the Dynamics of Thin Glassy Films

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements are simple high-throughput characterization experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glassy states for a variety of glassy materials. This technique allows for these parameters to be measured in a single experiment, while other methods must combine a variety of different techniques to investigate all of these properties. Measurements of dynamics close to Tg are particularly challenging. The advantage of cooling rate dependent Tg measurements over other methods which directly probe bulk and surface relaxation dynamics is that they are relatively quick and simple experiments, which do not utilize fluorophores or other complicated experimental techniques. Furthermore, this technique probes the average dynamics of technologically relevant thin films in temperature and relaxation time (&#964;&#945;) regimes relevant to the glass transition (&#964;&#945; &#62; 100 sec). The limitation to using ellipsometry for cooling rate dependent Tg experiments is that it cannot probe relaxation times relevant to measurements of viscosity (&#964;&#945; &#60;&#60; 1 sec). Other cooling rate dependent Tg measurement techniques, however, can extend the CR-Tg method to faster relaxation times. Furthermore, this technique can be used for any glassy system so long as the integrity of the film remains throughout the experiment.

Here, we present a protocol for cooling rate dependent ellipsometry experiments, which can determine the glass transition temperature (Tg), average dynamics, fragility and the expansion coefficient of the super-cooled liquid and glass for a variety of glassy materials.

薄いガラス質膜のダイナミクスを決定するレート依存エリプソメトリー測定を冷却

This report aims to fully describe the experimental technique of using ellipsometry for cooling rate dependent Tg (CR-Tg) experiments. These measurements ...

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 ...

Capillary Electrophoresis to Monitor Peptide Grafting onto Chitosan Films in Real Time

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. Compared to other analytical separation techniques, such as chromatography, CE is cheap, robust and effectively requires no sample preparation (for a number of complex natural matrices or polymeric samples). CE is fast and can be used to follow the evolution of mixtures in real time (e.g., chemical reaction kinetics), as the signals observed for the separated compounds are directly proportional to their quantity in solution.
Here, the efficiency of CE is demonstrated for monitoring the covalent grafting of peptides onto chitosan films for subsequent biomedical applications. Chitosan&#39;s antimicrobial and biocompatible properties make it an attractive material for biomedical applications such as cell growth substrates. Covalently grafting the peptide RGDS (arginine - glycine - aspartic acid - serine) onto the surface of chitosan films aims at improving cell attachment. Historically, chromatography and amino acid analysis have been used to provide a direct measurement of the amount of grafted peptide. However, the fast separation and absence of sample preparation provided by CE enables equally accurate yet real-time monitoring of the peptide grafting process. CE is able to separate and quantify the different components of the reaction mixture: the (non-grafted) peptide and the chemical coupling agents. In this way the use of CE results in improved films for downstream applications.
The chitosan films were characterized through solid-state NMR (nuclear magnetic resonance) spectroscopy. This technique is more time-consuming and cannot be applied in real time, but yields a direct measurement of the peptide and thus validates the CE technique.

Free solution capillary electrophoresis is a fast, cheap and robust analytical method that enables the quantitative monitoring of chemical reactions in real time. Its utility for rapid, convenient and precise analysis is demonstrated here through analysis of covalent peptide grafting onto chitosan films for improved cell adhesion.

リアルタイムでのキトサンフィルム上にペプチドグラフトを監視するためのキャピラリー電気泳動

Free-solution capillary electrophoresis (CE) separates analytes, generally charged compounds in solution through the application of an electric field. ...

Fabrication and Testing of Photonic Thermometers

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being leveraged for developing sophisticated photonic sensors. Silicon photonic sensors seek to exploit the strong confinement of light in nano-waveguides to transduce changes in physical state to changes in resonance frequency. In the case of thermometry, the thermo-optic coefficient, i.e., changes in refractive index due to temperature, causes the resonant frequency of the photonic device such as a Bragg grating to drift with temperature. We are developing a suite of photonic devices that leverage recent advances in telecom compatible light sources to fabricate cost-effective photonic temperature sensors, which can be deployed in a wide variety of settings ranging from controlled laboratory conditions, to the noisy environment of a factory floor or a residence. In this manuscript, we detail our protocol for the fabrication and testing of photonic thermometers.

We describe the process of fabrication and testing of photonic thermometers.

光温度計の作製と試験

In recent years, a push for developing novel silicon photonic devices for telecommunications has generated a vast knowledge base that is now being ...

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 ...