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.

Lesen Sie MSDS für Reagenzien und befolgen Sie alle chemischen Sicherheitsmaßnahmen gemäß Ihrer Institution.
(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>FeCl3, 97%</td>
			<td>Sigma Aldrich</td>
			<td>157740</td>
			<td></td>
		</tr>
		<tr>
			<td>Br2</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

33.5K 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

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 ...

Chemical Vapor Deposition of an Organic Magnet, Vanadium Tetracyanoethylene

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in traditional materials, including low cost and mechanical flexibility. In a similar vein, it would be advantageous to expand the use of organics into high frequency electronics and spin-based electronics. This work presents a synthetic process for the growth of thin films of the room temperature organic ferrimagnet, vanadium tetracyanoethylene (V[TCNE]x, x~2) by low temperature chemical vapor deposition (CVD). The thin film is grown at &#60;60 &#176;C, and can accommodate a wide variety of substrates including, but not limited to, silicon, glass, Teflon and flexible substrates. The conformal deposition is conducive to pre-patterned and three-dimensional structures as well. Additionally this technique can yield films with thicknesses ranging from 30 nm to several microns. Recent progress in optimization of film growth creates a film whose qualities, such as higher Curie temperature (600 K), improved magnetic homogeneity, and narrow ferromagnetic resonance line-width (1.5 G) show promise for a variety of applications in spintronics and microwave electronics.

We present the synthesis of the organic-based ferrimagnet vanadium tetracyanoethylene (V[TCNE]x, x~2) via low temperature chemical vapor deposition (CVD). This optimized recipe yields an increase in Curie temperature from 400 K to over 600 K and a dramatic improvement in magnetic resonance properties.

Chemical Vapor Deposition eines Organic Magnet, Vanadium Tetracyanethylen

Recent progress in the field of organic materials has yielded devices such as organic light emitting diodes (OLEDs) which have advantages not found in ...

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 ...

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

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

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

Herstellung von makroporösen Epitaxial-Quarz-Films auf Silizium durch Chemical Solution Deposition

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

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.

Kapillarelektrophorese zum Monitor Peptid Verpflanzen auf Chitosanfilme in Echtzeit

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

Low Pressure Vapor-assisted Solution Process for Tunable Band Gap Pinhole-free Methylammonium Lead Halide Perovskite Films

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, we present a protocol for the fabrication of this material via the low-pressure vapor assisted solution process (LP-VASP) method, which yields ~19% power conversion efficiency in planar heterojunction perovskite solar cells. First, we report the synthesis of methylammonium iodide (CH3NH3I) and methylammonium bromide (CH3NH3Br) from methylamine and the corresponding halide acid (HI or HBr). Then, we describe the fabrication of pinhole-free, continuous methylammonium-lead halide perovskite (CH3NH3PbX3 with X = I, Br, Cl and their mixture) films with the LP-VASP. This process is based on two steps: i) spin-coating of a homogenous layer of lead halide precursor onto a substrate, and ii) conversion of this layer to CH3NH3PbI3-xBrx by exposing the substrate to vapors of a mixture of CH3NH3I and CH3NH3Br at reduced pressure and 120 &#176;C. Through slow diffusion of the methylammonium halide vapor into the lead halide precursor, we achieve slow and controlled growth of a continuous, pinhole-free perovskite film. The LP-VASP allows synthetic access to the full halide composition space in CH3NH3PbI3-xBrx with 0&#160;&#8804; x&#160;&#8804; 3. Depending on the composition of the vapor phase, the bandgap can be tuned between 1.6 eV&#160;&#8804; Eg&#160;&#8804; 2.3 eV. In addition, by varying the composition of the halide precursor and of the vapor phase, we can also obtain CH3NH3PbI3-xClx. Films obtained from the LP-VASP are reproducible, phase pure as confirmed by X-ray diffraction measurements, and show high photoluminescence quantum yield. The process does not require the use of a glovebox.

Here, we present a protocol for the synthesis of CH3NH3I and CH3NH3Br precursors and the subsequent formation of pinhole-free, continuous CH3NH3PbI3-xBrx thin films for the application in high efficiency solar cells and other optoelectronic devices.

Dampf-gestützte Lösung Niederdruckverfahren für durchstimmbare Band Gap Pinhole-frei Methylammonium Blei Halogenid Perowskit Filme

Organo-lead halide perovskites have recently attracted great interest for potential applications in thin-film photovoltaics and optoelectronics. Herein, ...

Aerosol-assisted Chemical Vapor Deposition of Metal Oxide Structures: Zinc Oxide Rods

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, their high cost production and/or incompatibility with microfabrication technologies, due to the use of pre-deposited catalyst-seeds and/or high processing temperatures exceeding 900 &#176;C, represent a drawback for a widespread use of these methods. Here, however, we report the synthesis of ZnO rods via a non-catalyzed vapor-solid mechanism enabled by using an aerosol-assisted chemical vapor deposition (CVD) method at 400 &#176;C with zinc chloride (ZnCl2) as the precursor and ethanol as the carrier solvent. This method provides both single-step formation of ZnO rods and the possibility of their direct integration with various substrate types, including silicon, silicon-based micromachined platforms, quartz, or high heat resistant polymers. This potentially facilitates the use of this method at a large-scale, due to its compatibility with state-of-the-art microfabrication processes for device manufacture. This report also describes the properties of these structures (e.g., morphology, crystalline phase, optical band gap, chemical composition, electrical resistance) and validates its gas sensing functionality towards carbon monoxide.

Columnar zinc oxide structures in the form of rods are synthesized via aerosol-assisted chemical vapor deposition without the use of pre-deposited catalyst-seed particles. This method is scalable and compatible with various substrates based on either silicon, quartz or polymers.

Aerosol-assisted Chemical Vapor Deposition von Metall-Oxid-Strukturen: Zinkoxid-Stangen

Whilst columnar zinc oxide (ZnO) structures in the form of rods or wires have been synthesized previously by different liquid- or vapor-phase routes, ...

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

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

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

Überwachung der Auswirkungen der Beleuchtung auf die Struktur des konjugierten Polymer-Gel mit Neutronenstreuung

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

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

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

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

Raman und IR Spectroelectrochemical Methoden als Werkzeuge konjugierte organische Verbindungen zu analysieren

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