Name: reactive vapor deposition of conjugated polymer films on arbitrary substrates
Uploaded: 2018-01-17T10:55:00.000+00:00
Duration: 7 min 32 s
Description: Watch this Scientific Journal Video about Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates at JoVE.com

Die Autoren erkennen dankbar finanziellen Unterstützung durch die uns Air Force Office of Scientific Research, unter Vertragsnummer FA9550-14-1-0128. T. L. A. erkennt auch dankbar teilweise Unterstützung von David und Lucille Packard Foundation.

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(1) Ablagerung von Cl-PProDOT und Cl-PTT
<ol><li>Bauen Sie die Struktur der Custom-Built röhrenförmigen Dampf Deposition Kammer wie in Abbildung 1dargestellt.<ol>
<li>Machen Sie eine 1/4-Zoll (Außendurchmesser, O.D) verschmolzen Quarz Seiteneinlauf zu einem 2-Zoll (O.D) Quarzglas Schlauch. Machen Sie eine Kühlfalle mit einem speziell angefertigten U-Form 1-Zoll Edelstahl-Rohr und einem Dewar-Kolben.</li>
		<li>Schließen Sie das Quarzrohr mit Vakuummeter und Kühlfalle mit Edelstahl-KF Steckern und Quick-connect-Kupplungen. Das Monomer einen Quarz-Ampulle und anschließen die Ampulle der röhrenförmigen Kammer über 1/4-Zoll schnell-Anschluß-Kupplungen und ein Nadelventil. Legen Sie das Oxidationsmittel in einem Tiegel in der Kammer.</li>
		<li>Verwenden Sie separate Heizbänder als Wärmequellen für das Oxidationsmittel, Substrate und das Monomer. Fügen Sie ein Gaszutritt am rechten Ende der Kammer, weitere Edelgase zur Steuerung der Prozessdruck bei Bedarf einzuführen.</li>
	</ol>
</li>
	<li>
Ablagerung von Cl-PProDOT
	<ol>
<li>Fügen Sie 50 mg von 3,4-Propylenedioxythiophene (ProDOT) in der Monomer-Ampulle und verbinden Sie es mit der röhrenförmigen Kammer. Halten Sie das Nadel-Ventil offen.</li>
		<li>Setzen Sie Substrate (Objektträger, Stoffe, Papier, etc.) in der Kammer. Die Größe der Substrate ist 1,3 cm x 2,5 cm.</li>
		<li>Fügen Sie 50 mg von FeCl3 in einem 5-mL-Tiegel und legen Sie sie in die Kammer. Hinweis: Die relativen Positionen der Monomer-Einlass, Substrate und der Tiegel sind in Abbildung 1dargestellt. Der Abstand zwischen dem Monomer Zulauf und der Tiegel beträgt 13 cm.</li>
		<li>Schalten Sie die Pumpe. Schließen Sie das Ventil am rechten Ende der Kammer langsam. Nach der Kammer Druck liegt unter 525 mTorr (70 Pa), flüssigen Stickstoff in die Kühlfalle hinzufügen.</li>
		<li>Wickeln Sie die drei Heizzonen mit Heizleitung und verbinden Sie das Heizband mit dem Temperaturregler.</li>
		<li>Wenn der Druck sinkt auf der Verarbeitung Druck (52,5 mTorr, 7 Pa), schließen Sie das Nadel-Ventil des Behälters Monomer.</li>
		<li>Beginnen Sie das Oxidationsmittel, Substrate und das Monomer bei 170 ° C, 80 ° C und 80 ° C, bzw. Heizung. Nach ~ 10 min FeCl3 verdampft und die rote FeCl3 Feste in der kühlen Region gebildet wird.</li>
		<li>Öffnen Sie das Nadelventil des Behälters Monomer. Hinweis: Blau gefärbten dünne Folien werden im Bereich Substrat gebildet. Typische Wachstumsraten sind ~ 10 nm/min. sorgen dafür, dass die FeCl3 Dampf in die Kammer gebildet wird, vor dem Öffnen des Nadelventils des Behälters Monomer. Andernfalls wird das Monomer reagieren mit FeCl3 Feste in den Tiegel und bilden eine Polymerschicht verhindert die weitere Verdampfung des Oxidationsmittels.</li>
		<li>Schließen Sie das Nadelventil des Behälters Monomer, wenn die gewünschte Dicke erreicht ist. Schalten Sie alle Heizband und lassen Sie das System auf Raumtemperatur abkühlen.</li>
		<li>Öffnen Sie das Gas-Einlassventil und schalten Sie die Pumpe.</li>
		<li>Nehmen Sie die Proben aus der Kammer. Tauchen Sie vorsichtig die Proben in Methanol für 30 min die restlichen Oxidationsmittel und Monomer entfernen. Hinweis: Die Spülzeit sollte als Film Dicke erhöht erhöhen. 30-min Spülen ist typisch für Filme, die dünner als 100 nm auf Objektträgern. Filme dicker als 500 nm kann Delaminieren vom Substrat beim Spülen.</li>
		<li>Vorsichtig Föhnen die Proben mit Stickstoffgas.</li>
	</ol>
</li>
	<li>
Ablagerung von Cl-PTT
	<ol>
<li>Fügen Sie 50 mg von Thieno [3,2 -b] Thiophen (TT) in der Monomer-Ampulle und verbinden Sie es mit der röhrenförmigen Kammer. Halten Sie das Nadel-Ventil offen.</li>
		<li>Wiederholen Sie die Schritte 1.2.2. zu 1.2.12.</li>
	</ol>
</li>
</ol>2. Ablagerung von Br-PEDOT
<ol><li>
Ablagerung Kammer Setup
	<ol>
<li>Das Quarzrohr einen zusätzlichen 1/4-Zoll-Seite Einlass für Oxidantien hinzu und machen Sie es 8 Zoll neben dem Monomer-Einlass. Das flüssige Oxidationsmittel ein Quarz-Ampulle und schließen Sie die Ampulle der röhrenförmigen Kammer genauso wie das Monomer (Abbildung 2 an).</li>
	</ol>
</li>
	<li>
Ablagerung von Br-PEDOT
	<ol>
<li>Fügen Sie 2 mL von 3,4-Ethylenedioxythiophene (EDOT) in das Monomer-Ampulle und verbinden Sie die Ampulle mit der röhrenförmigen Kammer. Halten Sie das Nadel-Ventil offen.</li>
		<li>Legen Sie Substrate (Objektträger, Stoffe, Papier, etc.) in die röhrenförmigen Kammer in der Nähe der Monomer-Dampf-Einlass. Die Größe des Substrats ist 1,3 cm x 2,5 cm.</li>
		<li>In einer Dampfhaube Oxidationsmittel Ampulle 2 mL Br2 Add-in, verbinden Sie die Ampulle mit dem Nadelventil und das Nadelventil geschlossen zu halten. Schließen Sie das Nadelventil an das Quarzrohr. Vorsicht: BR2 ist ein Gefahrgut. Vorsicht beim Umgang mit.</li>
		<li>Schalten Sie die Pumpe. Schließen Sie das Ventil am rechten Ende der Kammer langsam. Nach der Kammer Druck liegt unter 525 mTorr (70 Pa), flüssigen Stickstoff in die Kühlfalle hinzufügen.</li>
		<li>Wickeln Sie die Monomer-Region mit Heizleitung und verbinden Sie es mit einem Temperaturregler. Halten Sie die Substrat und Oxidationsmittel Region bei Raumtemperatur.</li>
		<li>Wenn der Druck verringert die Verarbeitung Druck von 52,5 mTorr (7 Pa), öffnen Sie das Nadelventil des Oxidationsmittels. Hinweis: Die Reaktion ist sehr schnell. Blaue PEDOT Filme werden in der Nähe der Monomer-Einlass bilden, denn Br2 sehr volatil.</li>
		<li>Schließen Sie den Nadelventilen das Monomer und das Oxidationsmittel, wenn gewünschte Dicke erreicht ist.</li>
		<li>Schalten Sie das Heizband und lassen Sie das System auf Raumtemperatur abkühlen.</li>
		<li>Öffnen Sie das Gas-Einlassventil und schalten Sie die Pumpe. Nehmen Sie die Proben aus der Kammer. Hinweis: Spülen ist nicht erforderlich für Br2-dotierten Polymere.</li>
	</ol>
</li>
</ol>

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Die Autoren haben nichts preisgeben.

Der Mechanismus der Reaktion ist oxidative Polymerisation. Polymer-Beschichtung-Methoden mit dem gleichen Mechanismus gehören Electropolymerization17 und Dampf Phase Polymerisation18. Electropolymerization erfordert eine leitfähige Substrat, den Vorteil des einheitlichen und konforme Beschichtung fehlt, und ist eine umweltschädliche lösungsorientierte Methode19. Die bestehenden Dampf Phase Polymerisation Methode ist ähnlich der Methode hier beri...

Durchführung von Polymeren und halbleitenden Materialien haben einzigartige Eigenschaften, wie Flexibilität1, Dehnbarkeit2, Transparenz3und niedriger Dichte,4 die außergewöhnliche Möglichkeiten für die Erstellung von bieten nächsten Generation elektronischen Geräten auf untraditionelle Substrate. Derzeit sind viele Forscher bestrebt, die einzigartigen Eigenschaften von Polymeren Materialien flexibel erstellen und/oder wearable-Electronics-5,-6 und smarte Textilien7nutzen. Die Fähigkeit zur conformally stark strukturierte Oberflächen und nicht robust Substraten, wie Papier, Stoffen und Fäden/Garne, Beschichtung bleibt jedoch. Am häufigsten sind Polymere synthetisiert und auf Flächen mit Lösungsverfahren beschichtet. 8 , 9 , 10 , 11 , 12 obwohl Lösungsverfahren Polymer beschichtet Fasern/Textilien bieten, sind die so erhaltenen Beschichtungen oft nicht gleichmäßig und leicht beschädigt durch kleinen körperlichen Belastungen13,14 . Lösungsverfahren gelten auch nicht für Papierbeschichtung wegen Benetzung Probleme.
Reaktiven Aufdampfen kann auf den unterschiedlichsten Substraten, unabhängig von Chemie die Zusammensetzung Oberfläche, Oberflächenenergie und Rauheit/Oberflächentopographie15winkeltreue konjugierte Polymerfilme erstellen. Bei diesem Ansatz sind konjugierte Polymere in der Dampfphase synthetisiert, indem gleichzeitig Monomer und Oxidationsmittel Dämpfe an eine Oberfläche liefert. Polymerisation und Film Bildung erfolgt auf der Oberfläche in einem einzigen, lösemittelfreie Schritt. Diese Methode gilt theoretisch für alle konjugierten Polymer, das durch oxidative Polymerisierung mit Lösungsmethoden synthetisiert werden kann. Bislang sind jedoch Protokolle für die Hinterlegung nur einer schmale Reihe von konjugierten Polymer Strukturen bekannt. 15
Hier zeigen wir die Ablagerung von leitfähigen poly(3,4-ethylenedioxythiophene) (PEDOT) und poly(3,4-propylenedioxythiophene) (PProDOT) und halbleitenden Poly (Thieno [3,2 -b] Thiophen) (PTT) Filme über reaktiven Aufdampfen. Dabei sind zwei Arten von Oxidantien, solide FeCl3 und flüssigen Br2, genutzt. Die entsprechenden Polymere sind Cl-PProDOT, Cl-PTT und Br-PEDOT benannt. Sowohl konventionelle Substrate, Glas-Objektträger und unkonventionelle texturierten Substraten, wie Papier, Handtücher und Stoffe wurden mit Polymerfolien beschichtet.
Dieses Protokoll beschreibt die Einrichtung der Custom-Built Vapor Deposition Kammer und die Einzelheiten der Abscheidung. Es soll helfen, neue Praktiker ihre Ablagerung Buildsystem und vermeiden häufige Probleme mit Dampfphase Synthese verbunden.

<table><tbody><tr><td>3,4-Ethylenedioxythiophene, 97%</td><td>Sigma Aldrich</td><td>483028</td><td></td></tr><tr><td>3,4-Propylenedioxythiophene, 97%</td><td>Sigma Aldrich</td><td>660485</td><td></td></tr><tr><td>Thieno[3,2-b]thiophene, 95%</td><td>Sigma Aldrich</td><td>702668</td><td></td></tr><tr><td>FeCl&lt;sub&gt;3&lt;/sub&gt;, 97%</td><td>Sigma Aldrich</td><td>157740</td><td></td></tr><tr><td>Br&lt;sub&gt;2&lt;/sub&gt;</td><td>Sigma Aldrich</td><td>207888</td><td></td></tr></tbody></table>

reactive vapor deposition of conjugated polymer films on arbitrary substrates

Wir zeigen eine Methode conformally konjugierte Polymere auf beliebigen Substraten mit einer maßgeschneiderten, Niederdruck Reaktionskammer zu beschichten. Leitfähige Polymere, poly(3,4-ethylenedioxythiophene) (PEDOT) und poly(3,4-propylenedioxythiophene) (PProDOT), und eine halbleitende Polymere, Poly (Thieno [3,2 -b] Thiophen) (PTT), auf unkonventionelle abgelagert wurden, sehr ungeordnet und texturierten Substraten mit hohen Flächen wie Papier, Handtücher und Gewebe. Dies berichtet Ablagerung Kammer ist eine Verbesserung der bisherigen Dampf-Reaktoren, weil unser System flüchtigen und nichtflüchtigen Monomere wie 3,4-Propylenedioxythiophene und Thieno aufnehmen kann [3,2 -b] Thiophen. Verwertung von festen und flüssigen Oxidantien sind auch gezeigt. Eine Einschränkung dieser Methode ist, dass es anspruchsvoll in Situ Dicke Monitore fehlt. Polymerbeschichtungen gemacht durch die häufig verwendete lösungsorientierter Beschichtungsverfahren, wie Spin-Coating und Oberflächen zu veredeln, sind oft nicht einheitlich oder anfällig für mechanische Abbau. Dies berichtet Vapor Phase Abscheidungsverfahren überwindet diese Nachteile und ist eine starke Alternative zu gemeinsamen Lösung basierende Beschichtungsverfahren. Insbesondere sind Polymerfolien beschichtet durch die gemeldeten Methode einheitlich und winkeltreue auf rauen Oberflächen, auch bei einer Mikrometer Skala. Mit dieser Funktion können für zukünftige Anwendung von Dampf hinterlegt Polymeren in Geräten der Unterhaltungselektronik auf flexibel und stark strukturierte Untergründe.

Die Dicke der Cl-PProDOT Filme auf 1,3 x 2,5 cm Glas-Objektträger auf diskrete seitlichen Positionen entlang dem Zentralrohr gesetzt gebildet wurden durch ein Profilometer (Abbildung 3) gemessen. Leitfähigkeiten wurden von Widerstandsmessungen Messungen mit einer selbstgebauten Vierpunkt-Sonde-Teststation berechnet. Die gemessene Leitfähigkeit eines 100 nm dicken Cl-PProDOT Films auf Objektträgern ist 106 S/cm, die ausreicht, um diesen Film als eine mögl...

Watch this Scientific Journal Video about Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates at JoVE.com

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

Reaktiven Aufdampfen von konjugierten Polymerfilmen auf beliebigen Substraten

Dieser Beitrag stellt ein Protokoll für die reaktiven Aufdampfen von poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene) und Poly (Thieno [3,2 -b] Thiophen) Filme auf Objektträger und rauen Substraten, wie Textilien und Papier.

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

reactive-vapor-deposition-conjugated-polymer-films-on-arbitrary

Research

JoVE Journal

Chemistry

33.7K Aufrufe.  University of Wisconsin-Madison. Dieser Beitrag stellt ein Protokoll für die reaktiven Aufdampfen von poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene) und Poly (Thieno [3,2 -b] Thiophen) Filme auf Objektträger und rauen Substraten, wie Textilien und Papier.

Serie: Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

Preparation of Hydrophobic Metal-Organic Frameworks via Plasma Enhanced Chemical Vapor Deposition of Perfluoroalkanes for the Removal of Ammonia

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high surface area microporous materials, such as metal-organic frameworks (MOFs), unique challenges present themselves for PECVD treatments. Herein the protocol for development of a MOF that was previously unstable to humid conditions is presented. The protocol describes the synthesis of Cu-BTC (also known as HKUST-1), the treatment of Cu-BTC with PECVD of perfluoroalkanes, the aging of materials under humid conditions, and the subsequent ammonia microbreakthrough experiments on milligram quantities of microporous materials. Cu-BTC has an extremely high surface area (~1,800 m2/g) when compared to most materials or surfaces that have been previously treated by PECVD methods. Parameters such as chamber pressure and treatment time are extremely important to ensure the perfluoroalkane plasma penetrates to and reacts with the inner MOF surfaces. Furthermore, the protocol for ammonia microbreakthrough experiments set forth here can be utilized for a variety of test gases and microporous materials.

Herein the procedures for plasma enhanced chemical vapor deposition of perfluoroalkanes on microporous materials such as metal-organic frameworks to enhance their stability and hydrophobicity are described. Furthermore, breakthrough testing of milligram quantities of samples is described in detail.

Herstellung von hydrophoben Metall-organische Gerüste über Plasma Enhanced Chemical Vapor Deposition von Perfluoralkanen für die Beseitigung von Ammoniak

Plasma enhanced chemical vapor deposition (PECVD) of perfluoroalkanes has long been studied for tuning the wetting properties of surfaces. For high ...

Forschung

Chemie

Reductive Electropolymerization of a Vinyl-containing Poly-pyridyl Complex on Glassy Carbon and Fluorine-doped Tin Oxide Electrodes

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is one surface modification technique that electrodeposits a polymeric film at the surface of an electrode by utilizing an applied potential to initiate the polymerization of substrates in the Helmholtz layer. This useful technique was first established by a Murray-Meyer collaboration at the University of North Carolina at Chapel Hill in the early 1980s and utilized to study numerous physical phenomena of films containing inorganic complexes as the monomeric substrate. Here, we highlight a procedure for coating electrodes with an inorganic complex by performing reductive electropolymerization of the vinyl-containing poly-pyridyl complex onto glassy carbon and fluorine doped tin oxide coated electrodes. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization but are far less sensitive to oxygen and water.

A procedure for performing reductive electropolymerization of vinyl-containing compounds onto glassy carbon and fluorine doped tin-oxide coated electrodes is presented. Recommendations on electrochemical cell configurations and troubleshooting procedures are included. Although not explicitly described here, oxidative electropolymerization of pyrrole-containing compounds follows similar procedures to vinyl-based reductive electropolymerization.

Reduktive Elektropolymerisation eines Vinyl-enthaltenden Poly-pyridyl Komplexe des Glaskohlenstoffs und fluordotiertem Zinnoxidelektroden

Controllable electrode surface modification is important in a number of fields, especially those with solar fuels applications. Electropolymerization is ...

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.

Herstellung von großflächigen Freistehende ultradünne Polymerfilme

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

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.

Layer-by-Layer-Synthese und Übertragung von Freestanding konjugierte mikroporöse Polymernanomembranen

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

Atom Transfer Radical Polymerization of Functionalized Vinyl Monomers Using Perylene as a Visible Light Photocatalyst

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The procedure is performed under an inert atmosphere using air- and water-exclusion techniques. The outcome of the polymerization is affected by the ratios of monomer, initiator, and catalyst used as well as the reaction concentration, solvent, and nature of the light source. Temporal control over the polymerization can be exercised by turning the visible light source off and on. Low dispersities of the resultant polymers as well as the ability to chain-extend to form block copolymers suggest control over the polymerization, while chain end-group analysis provides evidence supporting an atom-transfer radical polymerization mechanism.

A method for the atom transfer radical polymerization of functionalized vinyl monomers using perylene as a visible-light photocatalyst is described.

Atomübertragungsradikalpolymerisation funktionalisierter Vinylmonomeren Mit Perylen als sichtbares Licht Photokatalysator

A standardized technique for atom transfer radical polymerization of vinyl monomers using perylene as a visible-light photocatalyst is presented. The ...

Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step process that finishes with Negishi coupling. Negishi coupling is a cross-coupling process in which a chemical precursor is first lithiated, followed by transmetallation with ZnCl2. The resultant organozinc compound can be coupled to a dibrominated aromatic precursor to give the conjugated monomer. Polymer films can be prepared via electropolymerization of the monomer and characterized using cyclic voltammetry and ultraviolet-visible-near infrared (UV-Vis-NIR) spectroscopy. Nanoparticles (NPs) are prepared via emulsion polymerization of the monomer using a two-surfactant system to yield an aqueous dispersion of the polymer NPs. The NPs are characterized using dynamic light scattering, electron microscopy, and UV-Vis-NIR-spectroscopy. Cytocompatibility of NPs is investigated using the cell viability assay. Finally, the NP suspensions are irradiated with a NIR laser to determine their effectiveness as potential materials for photothermal therapy (PTT).

A protocol is presented for the synthesis and preparation of nanoparticles consisting of electroactive polymers.

Elektroaktiven Polymer-Nanopartikel Teilnahmephotothermische Eigenschaften

A method for the synthesis of electroactive polymers is demonstrated, starting with the synthesis of extended conjugation monomers using a three-step ...

Ingenieurwesen

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.

Herstellung von reaktiven Oberflächen mit Pinsel-Like und querverbunden Filme von Azlactone funktionalisiert Block-Copolymere

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

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.

Verfahren zur Übertragung von Polymerfolien auf poröse Substrate mit minimierten Defekten

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

Development of Efficient OLEDs from Solution Deposition

The use of highly efficient organic emitters based on the thermally activated delayed fluorescence (TADF) concept is interesting due to their 100% internal quantum efficiency. Presented here is a solution deposition method for the fabrication of efficient organic light-emitting diodes (OLEDs) based on a TADF emitter in a simple device structure. This fast, low-cost, and efficient process can be used for all OLED emissive layers that follow the host-guest concept. The fundamental steps are described along with necessary information for further reproduction. The goal to establish a general protocol that can be easily adapted for principal organic emitters currently under study and development.

Presented here is a protocol for the fabrication of efficient, simple, solution-deposited organic light-emitting diodes with low roll-off.

Entwicklung effizienter OLEDs aus Solution Deposition

The use of highly efficient organic emitters based on the thermally activated delayed fluorescence (TADF) concept is interesting due to their 100% ...

Vapor Phase Deposition of Electroactive Poly(3,4-ethylenedioxythiophene) onto Electrospun Commodity Polymer Nanofibers

This study investigates the preparation of polyacrylonitrile (PAN) nanofibers through electrospinning to create highly porous and strong materials for applications in water purification, electrocatalysis, and biomedicine. The uniformly white PAN nanofiber mats were cut into 2 cm x 2 cm coupons to ensure consistency. After electrospinning, these nanofibers were coated with an electroactive polymer (EAP) using chemical vapor deposition, with iron (III) chloride (FeCl3) serving as an oxidant for polymerizing 3,4-ethylenedioxythiophene (EDOT) into poly(3,4-ethylenedioxythiophene) (PEDOT). The study examined the impact of different FeCl3 concentrations on PEDOT deposition on the PAN coupons. PEDOT deposition led to an increase in coupon weight. Scanning electron microscopy (SEM) revealed increases in the diameter of the nanofibers treated with increasing FeCl3 oxidant concentration, although higher FeCl3&#160;concentrations caused inter-fiber bridging, implying a concomitant decrease in inter-fiber spacing. Energy dispersive X-ray spectroscopy (EDS) was used to confirm the presence of Fe, Cl, and S in the nanofibers, with sulfur content rising with FeCl3&#160;concentration used, suggesting increased PEDOT deposition efficiency with increasing oxidant concentration. Mechanical testing showed that PEDOT-coated PAN fibers had improved tensile strength and toughness in the hydrated state compared to pure PAN nanofibers. These results highlight the crucial role of FeCl3&#160;concentration in influencing the morphology and properties of PAN-PEDOT composites, enhancing their suitability for applications such as water purification, tissue engineering, biosensing, catalysis, and energy storage.

This paper describes a simple technique for coating electrospun PAN nanofibers with electroactive polymers using vapor deposition. The effects of the oxidant FeCl&#8323; on the deposition of poly(3,4-ethylenedioxythiophene) coatings on PAN were investigated to understand and optimize polymer growth, fiber diameter, and overall mechanical strength of the nanofiber mats.

Dampfphasenabscheidung von elektroaktivem Poly(3,4-ethylendioxythiophen) auf elektrogesponnenen Polymer-Nanofasern

This study investigates the preparation of polyacrylonitrile (PAN) nanofibers through electrospinning to create highly porous and strong materials for ...