Name: fabrication of large-area free-standing ultrathin polymer films
Uploaded: 2015-06-03T14:00:00.000+00:00
Duration: 10 min 8 s
Description: Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

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><tbody><tr><td>Vinylec E</td><td>SPI</td><td></td><td></td></tr><tr><td>ethyl lactate, &gt;98%, FCC, FG</td><td>Sigma-Aldrich</td><td>W244007-1KG-K</td><td></td></tr><tr><td>4&quot; silicon wafers &amp;lt;100&gt;, 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&amp;nbsp;</td><td>WS-650-23</td><td></td></tr><tr><td>Barnstead/Thermolyne Super Nuova explosion-proof hot plate&amp;nbsp;</td><td></td><td></td><td></td></tr><tr><td>explosion-proof forced air oven</td><td>VWR&amp;nbsp;</td><td>1330 FMS&amp;nbsp;</td><td></td></tr><tr><td>balance with a range of 1&amp;nbsp;mg to 1,020&amp;nbsp;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&amp;nbsp;</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>1,000 ml beaker, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>60 ml glass vial with plastic stopper&amp;nbsp;</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&amp;nbsp;</td><td>PNHS-99</td><td></td></tr><tr><td>polyester knit 9/91 IPA/DI water wipes</td><td>Contec&amp;nbsp;</td><td>Prosat&amp;nbsp;</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 &amp;#956;m Luer-lock PTFE filters</td><td>Acrodisc&amp;nbsp;</td><td></td><td></td></tr><tr><td>0.45 &amp;#956;m Luer-lock PTFE filters</td><td>Acrodisc&amp;nbsp;</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

15.2K 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

Micropunching Lithography for Generating Micro- and Submicron-patterns on Polymer Substrates

Conducting polymers have attracted great attention since the discovery of high conductivity in doped polyacetylene in 19771. They offer the advantages of low weight, easy tailoring of properties and a wide spectrum of applications2,3. Due to sensitivity of conducting polymers to environmental conditions (e.g., air, oxygen, moisture, high temperature and chemical solutions), lithographic techniques present significant technical challenges when working with these materials4. For example, current photolithographic methods, such as ultra-violet (UV), are unsuitable for patterning the conducting polymers due to the involvement of wet and/or dry etching processes in these methods. In addition, current micro/nanosystems mainly have a planar form5,6. One layer of structures is built on the top surfaces of another layer of fabricated features. Multiple layers of these structures are stacked together to form numerous devices on a common substrate. The sidewall surfaces of the microstructures have not been used in constructing devices. On the other hand, sidewall patterns could be used, for example, to build 3-D circuits, modify fluidic channels and direct horizontal growth of nanowires and nanotubes.
A macropunching method has been applied in the manufacturing industry to create macropatterns in a sheet metal for over a hundred years. Motivated by this approach, we have developed a micropunching lithography method (MPL) to overcome the obstacles of patterning conducting polymers and generating sidewall patterns. Like the macropunching method, the MPL also includes two operations (Fig. 1): (i) cutting; and (ii) drawing. The "cutting" operation was applied to pattern three conducting polymers4, polypyrrole (PPy), Poly(3,4-ethylenedioxythiophen)-poly(4-styrenesulphonate) (PEDOT) and polyaniline (PANI). It was also employed to create Al microstructures7. The fabricated microstructures of conducting polymers have been used as humidity8, chemical8, and glucose sensors9. Combined microstructures of Al and conducting polymers have been employed to fabricate capacitors and various heterojunctions9,10,11. The "cutting" operation was also applied to generate submicron-patterns, such as 100- and 500-nm-wide PPy lines as well as 100-nm-wide Au wires. The "drawing" operation was employed for two applications: (i) produce Au sidewall patterns on high density polyethylene (HDPE) channels which could be used for building 3D microsystems12,13,14, and (ii) fabricate polydimethylsiloxane (PDMS) micropillars on HDPE substrates to increase the contact angle of the channel15.

A micropunching lithography approach is developed to generate micro- and submicron-patterns on top, sidewall and bottom surfaces of polymer substrates. It overcomes the obstacles of patterning conducting polymers and generating sidewall patterns. This method allows rapid fabrication of multiple features and is free of aggressive chemistry.

ポリマー基板上へのマイクロ·サブミクロンのパターンを生成するためのリソグラフィMicropunching

Conducting polymers have attracted great attention since the discovery of high conductivity in doped polyacetylene in 19771. They offer the advantages of ...

工学

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

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

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

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 ...

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.

任意の基板上への共役ポリマー薄膜の反応性蒸着

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

斜め蒸着を使用してメディアを高吸収極薄カラー フィルムの作製

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Fabricating Reactive Surfaces with Brush-like and Crosslinked Films of Azlactone-Functionalized Block Co-Polymers

In this paper, fabrication methods that generate novel surfaces using the azlactone-based block co-polymer, poly (glycidyl methacrylate)-block-poly (vinyl dimethyl azlactone) (PGMA-b-PVDMA), are presented. Due to the high reactivity of azlactone groups towards amine, thiol, and hydroxyl groups, PGMA-b-PVDMA surfaces can be modified with secondary molecules to create chemically or biologically functionalized interfaces for a variety of applications. Previous reports of patterned PGMA-b-PVDMA interfaces have used traditional top-down patterning techniques that generate non-uniform films and poorly controlled background chemistries. Here, we describe customized patterning techniques that enable precise deposition of highly uniform PGMA-b-PVDMA films in backgrounds that are chemically inert or that have biomolecule-repellent properties. Importantly, these methods are designed to deposit PGMA-b-PVDMA films in a manner that completely preserves azlactone functionality through each processing step. Patterned films show well-controlled thicknesses that correspond to polymer brushes (~90 nm) or to highly crosslinked structures (~1-10 &#956;m). Brush patterns are generated using either the parylene lift-off or interface directed assembly methods described and are useful for precise modulation of overall chemical surface reactivity by adjusting either the PGMA-b-PVDMA pattern density or the length of the VDMA block. In contrast, the thick, crosslinked PGMA-b-PVDMA patterns are obtained using a customized micro-contact printing technique and offer the benefit of higher loading or capture of secondary material due to higher surface area to volume ratios. Detailed experimental steps, critical film characterizations, and trouble-shooting guides for each fabrication method are discussed.

Surface fabrication methods for patterned deposition of nanometer thick brushes or micron thick, crosslinked films of an azlactone block co-polymer are reported. Critical experimental steps, representative results, and limitations of each method are discussed. These methods are useful for creating functional interfaces with tailored physical features and tunable surface reactivity.

ブラシのような反応性表面を加工し、アズラクトン官能基化ブロック共重合体の架橋膜

In this paper, fabrication methods that generate novel surfaces using the azlactone-based block co-polymer, poly (glycidyl methacrylate)-block-poly (vinyl ...

Thin Film Composite Silicon Elastomers for Cell Culture and Skin Applications: Manufacturing and Characterization

In this protocol, we present methods to fabricate thin elastomer composite films for advanced cell culture applications and for the development of skin adhesives. Two different poly-(dimethyl siloxanes) (PDMS and soft skin adhesive (SSA)), have been used for in depth investigation of biological effects and adhesive characteristics. The composite films consist of a flexible backing layer and an adhesive top coating. Both layers have been manufactured by doctor blade application technique. In the present investigation, the adhesive behavior of the composite films has been investigated as a function of the layer thickness or a variation of the Young&#39;s modulus of the top layer. The Young&#39;s modulus of PDMS has been changed by varying the base to crosslinker mixing ratio. In addition, the thickness of SSA films has been varied from approx. 16 &#181;m to approx. 320 &#181;m. Scanning electron microscopy (SEM) and optical microscopy have been used for thickness measurements. The adhesive properties of elastomer films depend strongly on the film thickness, the Young&#39;s modulus of the polymers and surface characteristics. Therefore, normal adhesion of these films on glass substrates exhibiting smooth and rough surfaces has been investigated. Pull-off stress and work of separation are dependent on the mixing ratio of silicone elastomers.
Additionally, the thickness of the soft skin adhesive placed on top of a supportive backing layer has been varied in order to produce patches for skin applications. Cytotoxicity, proliferation and cellular adhesion of L929 murine fibroblasts on PDMS films (mixing ratio 10:1) and SSA films (mixing ratio 50:50) have been conducted. We have shown here, for the first time, the side by side comparison of thin composite films manufactured of both polymers and present the investigation of their biological- and adhesive properties.

A protocol for the manufacturing process of polymeric thin film composite structures possessing either different Young&#39;s moduli or thicknesses is presented. Films are produced for advanced cell culture studies or as skin adhesives.

細胞培養および皮膚のアプリケーション フィルム複合シリコン エラストマーを薄い: 製造とキャラクタリゼーション

In this protocol, we present methods to fabricate thin elastomer composite films for advanced cell culture applications and for the development of skin ...

発生生物学

Procedure for the Transfer of Polymer Films Onto Porous Substrates with Minimized Defects

The fabrication of devices containing thin film composite membranes necessitates the transfer of these films onto the surfaces of arbitrary support substrates. Accomplishing this transfer in a highly controlled, mechanized, and reproducible manner can eliminate the creation of macroscale defect structures (e.g., tears, cracks, and wrinkles) within the thin film that compromise device performance and the usable area per sample. Here, we describe a general protocol for the highly controlled and mechanized transfer of a polymeric thin film onto an arbitrary porous support substrate for eventual use as a water filtration membrane device. Specifically, we fabricate a block copolymer (BCP) thin film on top of a sacrificial, water-soluble poly(acrylic acid) (PAA) layer and silicon wafer substrate. We then utilize a custom-designed, 3D-printed transfer tool and drain chamber system to deposit, lift-off, and transfer the BCP thin film onto the center of a porous anodized aluminum oxide (AAO) support disc. The transferred BCP thin film is shown to be consistently placed onto the center of the support surface due to the guidance of the meniscus formed between the water and the 3D-printed plastic drain chamber. We also compare our mechanized transfer-processed thin films to those that have been transferred by hand with the use of tweezers. Optical inspection and image analysis of the transferred thin films from the mechanized process confirm that little-to-no macroscale inhomogeneities or plastic deformations are produced, as compared to the multitude of tears and wrinkles produced from manual transfer by hand. Our results suggest that the proposed strategy for thin film transfer can reduce defects when compared to other methods across many systems and applications.

We present a procedure for highly controlled and wrinkle-free transfer of block copolymer thin films onto porous support substrates using a 3D-printed drain chamber. The drain chamber design is of general relevance to all procedures involving transfer of macromolecular films onto porous substrates, which is normally done by hand in an irreproducible fashion.

欠陥を最小限に抑えた多孔質基板へのポリマーフィルムの移送手順

The fabrication of devices containing thin film composite membranes necessitates the transfer of these films onto the surfaces of arbitrary support ...

A Femtoliter Droplet Array for Massively Parallel Protein Synthesis from Single DNA Molecules

Advances in spatial resolution and detection sensitivity of scientific instrumentation make it possible to apply small reactors for biological and chemical research. To meet the demand for high-performance microreactors, we developed a femtoliter droplet array (FemDA) device and exemplified its application in massively parallel cell-free protein synthesis (CFPS) reactions. Over one million uniform droplets were readily generated within a finger-sized area using a two-step oil-sealing protocol. Every droplet was anchored in a femtoliter microchamber composed of a hydrophilic bottom and a hydrophobic sidewall. The hybrid hydrophilic-in-hydrophobic structure and the dedicated sealing oils and surfactants are crucial for stably retaining the femtoliter aqueous solution in the femtoliter space without evaporation loss. The femtoliter configuration and the simple structure of the FemDA device allowed minimal reagent consumption. The uniform dimension of the droplet reactors made large-scale quantitative and time-course measurements convincing and reliable. The FemDA technology correlated the protein yield of the CFPS reaction with the number of DNA molecules in each droplet. We streamlined the procedures about the microfabrication of the device, the formation of the femtoliter droplets, and the acquisition and analysis of the microscopic image data. The detailed protocol with the optimized low running cost makes the FemDA technology accessible to everyone who has standard cleanroom facilities and a conventional fluorescence microscope in their own place.

The overall goal of the protocol is to prepare over one million ordered, uniform, stable, and biocompatible femtoliter droplets on a 1 cm2 planar substrate that can be used for cell-free protein synthesis.

単一DNA分子からの超並列タンパク質合成のためのフェムトリットルドロップレットアレイ

Advances in spatial resolution and detection sensitivity of scientific instrumentation make it possible to apply small reactors for biological and ...

A Simple and Scalable Fabrication Method for Organic Electronic Devices on Textiles

Today, wearable electronics devices combine a large variety of functional, stretchable, and flexible technologies. However, in many cases, these devices cannot be worn under everyday conditions. Therefore, textiles are commonly considered the best substrate to accommodate electronic devices in wearable use. In this paper, we describe how to selectively pattern organic electroactive materials on textiles from a solution in an easy and scalable manner. This versatile deposition technique enables the fabrication of wearable organic electronic devices on clothes.

In this paper, we present a protocol to selectively deposit organic materials on textiles, which allows for the direct integration of organic electronic devices with wearables. The fabricated devices can be fully integrated in textiles, respecting their mechanical appearance and enabling sensing capabilities.

テキスタイル上の有機電子デバイスのためのシンプルでスケーラブルな製造方法

Today, wearable electronics devices combine a large variety of functional, stretchable, and flexible technologies. However, in many cases, these devices ...

大面積自立超薄ポリマーフィルムの作製

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ポリマー基板上へのマイクロ·サブミクロンのパターンを生成するためのリソグラフィMicropunching

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

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

任意の基板上への共役ポリマー薄膜の反応性蒸着

斜め蒸着を使用してメディアを高吸収極薄カラーフィルムの作製

ブラシのような反応性表面を加工し、アズラクトン官能基化ブロック共重合体の架橋膜

細胞培養および皮膚のアプリケーションフィルム複合シリコンエラストマーを薄い: 製造とキャラクタリゼーション

欠陥を最小限に抑えた多孔質基板へのポリマーフィルムの移送手順

単一DNA分子からの超並列タンパク質合成のためのフェムトリットルドロップレットアレイ

テキスタイル上の有機電子デバイスのためのシンプルでスケーラブルな製造方法

大面積自立超薄ポリマーフィルムの作製

要約

さらに動画を探す

この動画の章

ポリマー基板上へのマイクロ·サブミクロンのパターンを生成するためのリソグラフィMicropunching

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

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

任意の基板上への共役ポリマー薄膜の反応性蒸着

斜め蒸着を使用してメディアを高吸収極薄カラー フィルムの作製

ブラシのような反応性表面を加工し、アズラクトン官能基化ブロック共重合体の架橋膜

細胞培養および皮膚のアプリケーション フィルム複合シリコン エラストマーを薄い: 製造とキャラクタリゼーション

欠陥を最小限に抑えた多孔質基板へのポリマーフィルムの移送手順

単一DNA分子からの超並列タンパク質合成のためのフェムトリットルドロップレットアレイ

テキスタイル上の有機電子デバイスのためのシンプルでスケーラブルな製造方法

斜め蒸着を使用してメディアを高吸収極薄カラーフィルムの作製

細胞培養および皮膚のアプリケーションフィルム複合シリコンエラストマーを薄い: 製造とキャラクタリゼーション