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

Questo lavoro svolto sotto l&#39;egida del Dipartimento dell&#39;Energia degli Stati Uniti da Lawrence Livermore National Laboratory sotto contratto DE-AC52-07NA27344.

1. Soluzione Preparazione <ol><li> Filtrare 60 g di lattato di etile utilizzando una siringa e un filtro a siringa da 0,20 micron. Aggiungere 0,3 g di polivinil formale al lattato di etile. Posizionare la soluzione in forno a 50 ° C per 4 ore. Agitare il flacone delicatamente per vedere se il polimero è completamente sciolta. <ol><li> Se la soluzione è torbida o ancora mostra disomogeneità ottica, riportare la fiala al forno per altri 2 ore. Questa ricetta è per una soluzione polimerica allo 0,5% in peso, che viene in genere utilizzato per spessori del film circa 30 nm. Soluzioni con maggiore contenuto in peso del polimero può essere utilizzato per pellicole più spesse. </li></ol></li><li> Preparare una soluzione PDAC pesando 1,0 g di PDAC reattivo in un pallone tarato da 20 ml e riempire il pallone linea di misurazione con acqua deionizzata (DI). Agitare delicatamente la soluzione prima di trasferirlo a un contenitore di stoccaggio. </li></ol> 2. Preparazione del supporto <ol><li> ATTENZIONE. Versare 60 ml di acido solforico concentratoacido in un becher da 250 ml pulito. Aggiungere lentamente 20 ml di 30% di perossido di idrogeno. Attendere fino a quando fumante placa, quindi agitare la soluzione delicatamente. La soluzione e il bicchiere diventerà molto caldo e la miscela è corrosiva. </li><li> Mettere una capsula di Petri 150 millimetri sulla piastra calda e versare l&#39;acido nel piatto. Impostare la piastra calda a 100 ° C. <ol><li> Inserire un wafer 4 &#39;di silicio nell&#39;acido con il lato lucido up. Spingere delicatamente il wafer nel mezzo con un paio di pinzette per assicurarsi che l&#39;intera superficie è bagnata. Lasciare il wafer nell&#39;acido per 30 min. </li></ol></li><li> Rimuovere il wafer dall&#39;acido con un paio di pinzette e sciacquare la parte anteriore e posteriore del wafer accuratamente con acqua deionizzata da una spruzzetta. L&#39;acqua dovrebbe lenzuolo in modo regolare. Asciugare il wafer in un banco pulito. </li><li> Risciacquare una siringa monouso 3 ml ed un filtro prima con acqua DI 0,2 um e quindi con soluzione PDAC disegnando il liquido nella siringa, montaggio del filtro, e lan spingere il liquido attraverso il filtro. </li><li> Montare un wafer pulito nel dispositivo a induzione di rotazione. Elaborare 1,0-1,2 ml di soluzione PDAC nella siringa ed erogare, però il filtro sul centro della cialda. Spin a 4.000 giri per 15 secondi, poi il trasferimento il wafer di un piatto caldo (preriscaldato a 50 ° C) e lasciare riposare per 30 sec. </li><li> Sciacquare il livello PDAC asciugato con acqua deionizzata e lasciare asciugare il wafer nel banco pulito. </li></ol> Fabrication 3. Film <ol><li> Posizionare un wafer PDAC trattato secco sul dispositivo a induzione di rotazione. </li><li> Risciacquare una siringa monouso da 3 ml e un filtro da 0,45 micron con la soluzione di lattato di etile utilizzando la procedura di cui 2.4). </li><li> Cassetta 2,5 ml della soluzione di lattato di etile attraverso il filtro con la siringa nel centro della cialda e centrifugare per 10 sec a 200 rpm, poi per 3 secondi a 1700 rpm (dipendente spessore del film desiderato). Ci dovrebbe essere un film liquido uniforme sul wafer. </li><li> Lasciate che il film secco del dispositivo a induzione di rotazionefino a quando è visibilmente secco (tipicamente 10-15 min), poi posto su una piastra (preriscaldata a 50 ° C) per 10 min. </li><li> Tagliare il film in quadrati più piccoli per il decollo, tipicamente 2 cm x 2 cm ma può essere più grande, a seconda delle dimensioni del supporto per pellicola utilizzata (3.5.1-3.5.2). In alternativa, fare due scribi per delaminazioni un film wafer di dimensioni (3.5.3). Nota: supporti per pellicola standard sono 19 x 19 mm, con un foro circolare di diametro di 13 mm nel mezzo. Per film wafer dimensioni, utilizzare un telaio di filo (ad esempio, filo di acciaio inossidabile formato in un cerchio) con un diametro da 1 &quot;più piccolo del wafer. Un&#39;apertura circolare è scelto perché i film in genere assorbire l&#39;acqua durante il decollo e si gonfiano. Come i film secchi sul supporto, l&#39;acqua viene rimossa e il film termoretraibile. Un&#39;apertura circolare permette una distribuzione uniforme delle sollecitazioni. <ol><li> Posizionare la cialda su un modello di taglio. Utilizzare un modello quadrato su cui tutti i bordi sono più alti rispetto alla cialda per evitare che il diritto eDGE utilizzato per guidare la lama durante scribing di toccare il wafer. Segna i bordi in intervalli di 2 centimetri per guidare il posizionamento del regolo durante dadi. Spingere la cialda contro due bordi per allinearlo. </li><li> Posizionare un regolo lungo due tacche di allineamento, e disegnare una lama di rasoio dolcemente lungo il regolo per incidere il film. Applicare una pressione sufficiente a marcare il film, ma non troppo per contrassegnare la cialda stessa e produrre particelle. Sul film spessi, la linea di taglio sarà chiaramente visibile. </li><li> Per decollata un film in un sol pezzo di wafer, scrivano bordo wafer con una lama di rasoio. Tra i due appartamenti al wafer, scriba una striscia larga abbastanza per bloccare il wafer sulla cremagliera e pignone. </li></ol></li><li> Riempire un piatto mm 190 x 100 cultura con acqua deionizzata. Bloccare il wafer dalla grande piana ad una cremagliera e pignone montato su un palcoscenico inclinazione e abbassare lentamente in acqua deionizzata. Il film dovrebbe separare dal wafer alla linea di galleggiamento. <ol><li> Continuare ad abbassare il wafer ad un tasso che conferisce al film tempo sufficiente per separare dal wafer, piuttosto che spingere l&#39;interfaccia lift-off di sotto della linea di galleggiamento. Quando la prima fila di caselle è distaccata dal wafer e galleggia sulla superficie, sospendere l&#39;abbassamento del wafer. Per un film di wafer di dimensioni, continuare immergendo il wafer finché la pellicola non si stacca completamente. </li><li> Immergere la testa del supporto per pellicola in acqua e spostarlo sotto la pellicola. Allineare il bordo maniglia del cerchio con uno dei bordi della pellicola e toccare il cerchio con il film. In caso di successo, il film si attacchi al cerchio. <ol><li> Per un film di wafer-size, posizionare il telaio di filo sotto la sezione descritto, solo un centimetro di distanza dal bordo. Assicurarsi che il telaio sia centrato sotto il film prima di iniziare la cattura, il mantenimento di una certa distanza tra il bordo della pellicola e il bordo del cerchio in modo che il film può avvolgere intorno al cerchio e ripiegare su se stessa. </li></ol></li><li> Ritrarre il cerchio lentamente dall&#39;acqua a unangolo di 35 °. Sollevare la pellicola fuori dall&#39;acqua molto lentamente. Nota: Per i film meno di 20 nm di spessore, aumentare l&#39;angolo dopo circa metà del film è stato tirato dall&#39;acqua a quasi 90 ° (cioè, normale alla superficie dell&#39;acqua) per evitare di tirare il film attraverso il supporto. Quando si cambia l&#39;angolo ascensore fuori, farlo lentamente per evitare di tirare il film attraverso il cerchio. </li><li> Quando il telaio è completamente retratto, posizionarlo a lato per asciugare. Assicurarsi che il fondo del cerchio è priva di gocce prima di mettere il cerchio verso il basso, e utilizzare una superficie curva (ad esempio un cassetto fetta) per evitare di creare una tenuta di liquido tra il telaio e la superficie. </li><li> Se piazze più tracciatura rimangono sul wafer, continua abbassando il wafer in acqua e ripetere i passaggi sopra per 3.6.1-3.6.4 piazze rimanenti. </li><li> Lasciate che i film O secco / N. </li></ol></li></ol>

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Il trattamento substrato PDAC si basa su interazioni elettrostatiche autolimitanti, cioè substrati di qualsiasi dimensione può essere facilmente trattato, purché siano caricate negativamente (ad esempio, silicio o vetro). Figure 1-2 mostra molto grandi film sottili (fino a 13 centimetri di diametro) fabbricati usando questo protocollo, con l&#39;unico cambiamento è il volume dei reagenti usati. La dimensione finale ottenibile sembra essere limitata solo dalle attrezzature deposizione e dela...

Free-standing film polimerici sottili sono utilizzati in una vasta gamma di applicazioni, tra cui sensori, 1-3 MEM, la catalisi o filtrazione, 4 e ingegneria dei tessuti. 5-8 sono utilizzati anche per studi fondamentali che esplorano il comportamento dei polimeri in ambiente confinato. 9- 13 Un film autoportante è uno che è supportato su un substrato non continua, come un anello o cerchio al contrario di un wafer di silicio o vetrino. Questo lavoro descrive una procedura semplice e ripetibile per la fabbricazione di film free-standing polimeri ultrasottili che è adatto per i film di grande superficie e produzione high-throughput. È compatibile con una varietà di diversi polimeri, tra poli (vinil formale), polistirene, e poli (metil metacrilato). Può essere usato per fabbricare pellicole autoportanti che sono grandi come diametro di 13 cm o più sottile 10 nm. La fabbricazione dei polimeri free-standing si compone di tre fasi fondamentali: 1) deposition del film polimerico su un substrato tradizionale come un wafer o slitta, 2) rilascio o decollo del film dal substrato, e 3) la cattura del film risultante su un supporto. Dettagli Questo articolo una procedura che abbiamo riportato in un precedente studio sui vari metodi di rilascio. 14 Deposizione può essere ottenuta con qualsiasi numero di tecnologie di base di polimeri film sottile come spin-coating, deposizione di vapore, o dip-coating. In questo lavoro, utilizziamo le tecniche di spin-rivestimento standard. Il &quot;float off-lift a&quot; tecnica è il metodo più comune per rilasciare un film ultrasottile dal suo substrato. 15 In questa tecnica, il film ed il substrato sono immersi in un bagno di solvente adatto. Il solvente si gonfia il film e induce delaminazione spontanea, rilasciando il film e che galleggi all&#39;inizio del bagno. Lo spessore minimo del film che puòessere rilasciato con lift off-galleggiante è determinata equilibrando l&#39;energia peeling interfacciale con l&#39;energia di deformazione gonfiore indotta: 16 <img alt="Equazione 1" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> (1) Dove L è lo spessore del film, ν f è il coefficiente di Poisson del film, E è il modulo di Young del film, ξ è il rapporto di rigonfiamento del film, e γ è l&#39;energia interfacciale di peeling. Il modo tipico per bypassare la limitazione imposta dalla equazione (1) è di depositare uno strato intermedio sacrificale tra il film ed il substrato di deposizione. 17-20 Quando questo interstrato dissolve in solvente, il film viene rilasciato e può essere catturato su un supporto . Un relativo metodo è il metodo sovrastrato sacrificale, che utilizza peeling meccanica del film su uno strato sacrificale prIOR alla dissoluzione. 21 L&#39;utilizzo di materiali sacrificali ha diversi svantaggi principali. In primo luogo, l&#39;aggiunta di un materiale di processo supplementare e passaggio potrebbe richiedere un compromesso tra le condizioni ottimali pellicola di fabbricazione ed alle condizioni di materiale sacrificale. In secondo luogo, i materiali sacrificali possono essere difficili da deposito senza alterare le proprietà meccaniche o la purezza del film free-standing finale. In terzo luogo, il procedimento per depositare il materiale sacrificale deve essere ottimizzato e monitorati per la qualità come un&#39;operazione nel free-standing pellicola fabbricazione complessiva. 14 In questo lavoro, si descrive una tecnica di modifica della superficie che riduce l&#39;energia peeling interfacciale, consentendo il decollo flottante sulla tecnica da utilizzare per i film ultrasottili. Il substrato di deposizione viene modificato con l&#39;assemblaggio di un auto-limitata, auto-ottimizzante quasi monostrato del cloruro policatione polydiallyldiammonium (PDAC). A causa dellaforza del legame tra il policatione e il substrato, questa modifica superficie è robusta a successive fasi di processo. La natura auto-limitante e di auto-ottimizzazione della formazione quasi monostrato richiede praticamente a zero l&#39;ottimizzazione ed è facilmente scalabile per grandi aree. Dopo la rimozione, il film galleggia alla parte superiore della vasca del solvente in cui viene catturato su un supporto telaio simile. Mentre non dato molta attenzione nella letteratura esistente, in questo lavoro si descrivono tecniche per catturare film di grande superficie su supporti che riducono la probabilità di strappo o altrimenti danneggiare la pellicola.

<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.

La Figura 1 mostra un esempio di una sottile pellicola polimerica autoportante su una vasta area. Questo polivinil film spesso formale a 55 nm è stato fabbricato utilizzando la procedura qui descritta ed è montato su un 13-cm cerchio d&#39;acciaio di diametro. La delaminazione avviene su grandi aree senza introdurre difetti che portano alla lacerazione della pellicola. Così, la resistenza intrinseca di polyvinylformal può essere sfruttata anche per pellicole molto sottili. La Figura 2</stron...

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.

Fabbricazione di ampia superficie Free-standing ultrasottili film polimerici

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 Views.  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.

Video: 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.

Micropunching litografia per la generazione di Micro-e submicroniche modelli sul Polymer Substrati

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

Ricerca

Ingegneria

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.

Verso Biomimicking Legno: Fabbricato Free-standing Films di Nanocellulose, lignina, e policatione sintetico

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

Chimica

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.

Sintesi layer-by-layer e di trasferimento delle Freestanding coniugati microporosi Polymer nanomembrane

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.

Deposizione di vapore reattiva di film polimerici coniugati su substrati arbitrari

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.

Fabbricazione di film ultra-sottile di colore con altamente assorbente Media mediante deposizione di angolo obliquo

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.

Fabbricazione di superfici reattive con spazzola e film reticolato di co-polimeri funzionalizzati Azlactone blocco

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.

Thin Film composito silicone elastomeri per colture cellulari e applicazioni della pelle: produzione e caratterizzazione

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

Biologia dello sviluppo

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.

Procedura per il trasferimento di pellicole polimeriche su substrati porous con difetti ridotti al minimo

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.

Un array di gocciole del femtolitro per sintesi proteica massicciamente parallela da molecole di DNA singolo

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.

Un metodo semplice e scalabile di fabbricazione per dispositivi elettronici organici sui tessili

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