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

fabrication of large-area free-standing ultrathin polymer films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films. Typically, ultrathin films are prepared using either sacrificial layers, which may damage the film or affect its mechanical properties, or they are made on freshly cleaved mica, a substrate that is difficult to scale. Further, the size of ultrathin film is typically limited to a few square millimeters. In this method, we modify a surface with a polyelectrolyte that alters the strength of adhesion between polymer and deposition substrate. The polyelectrolyte can be shown to remain on the wafer using spectroscopy, and a treated wafer can be used to produce multiple films, indicating that at best minimal amounts of the polyelectrolyte are added to the film. The process has thus far been shown to be limited in scalability only by the size of the coating equipment, and is expected to be readily scalable to industrial processes. In this study, the protocol for making the solutions, preparing the deposition surface, and producing the films is described.

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

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 ...

Ricerca

Chimica

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed assembly1-3, drug delivery4, improved hydrocarbon recovery5-7, and flowable electrodes for energy storage8. Suspensions containing fluorescent colloids and non-adsorbing polymers are appealing model systems, as the ratio of the polymer radius of gyration to the particle radius&#160;and concentration of polymer control the range and strength of the interparticle attraction, respectively. By tuning the polymer properties and the volume fraction of the colloids, colloid fluids, fluids of clusters, gels, crystals, and glasses can be obtained9.&#160;Confocal microscopy, a variant of fluorescence microscopy, allows an optically transparent and fluorescent sample to be imaged with high spatial and temporal resolution in three dimensions. In this technique, a small pinhole or slit blocks the emitted fluorescent light from regions of the sample that are outside the focal volume of the microscope optical system. As a result, only a thin section of the sample in the focal plane is imaged. This technique is particularly well suited to probe the structure and dynamics in dense colloidal suspensions at the single-particle scale: the particles are large enough to be resolved using visible light and diffuse slowly enough to be captured at typical scan speeds of commercial confocal systems10. Improvements in scan speeds and analysis algorithms have also enabled quantitative confocal imaging of flowing suspensions11-16,37.&#160;In this paper, we demonstrate confocal microscopy experiments to probe the confined phase behavior and flow properties of colloid-polymer mixtures. We first prepare colloid-polymer mixtures that are density- and refractive-index matched. Next, we report a standard protocol for imaging quiescent dense colloid-polymer mixtures under varying confinement in thin wedge-shaped cells. Finally, we demonstrate a protocol for imaging colloid-polymer mixtures during microchannel flow.

Confocal microscopy is used to image quiescent and flowing colloid-polymer mixtures, which are studied as model systems for attractive suspensions. Image analysis algorithms are used to calculate structural and dynamic metrics for the colloidal particles that measure changes due to geometric confinement.

Imaging confocale di confinati riposo e fluenti miscele colloidali e polimeri

The behavior of confined colloidal suspensions with attractive interparticle interactions is critical to the rational design of materials for directed ...

Preparation of Highly Porous Coordination Polymer Coatings on Macroporous Polymer Monoliths for Enhanced Enrichment of Phosphopeptides

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous polymer monoliths. The developed approach is based on the preparation of a macroporous polymer containing carboxylic acid functional groups and the subsequent step-by-step solution-based controlled growth of a layer of a porous coordination polymer on the surface of the pores of the polymer monolith. The prepared metal-organic polymer hybrid has a high specific micropore surface area. The amount of iron(III) sites is enhanced through metal-organic coordination on the surface of the pores of the functional polymer support. The increase of metal sites is related to the number of iterations of the coating process.
The developed preparation scheme is easily adapted to a capillary column format. The functional porous polymer is prepared as a self-contained single-block porous monolith within the capillary, yielding a flow-through separation device with excellent flow permeability and modest back-pressure. The metal-organic polymer hybrid column showed excellent performance for the enrichment of phosphopeptides from digested proteins and their subsequent detection using matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The presented experimental protocol is highly versatile, and can be easily implemented to different organic polymer supports and coatings with a plethora of porous coordination polymers and metal-organic frameworks for multiple purification and/or separation applications.

A procedure for the preparation of porous hybrid separation media composed of a macroporous polymer monolith internally coated by a high surface area microporous coordination polymer is presented.

Preparazione di altamente poroso Coordinamento rivestimenti polimerici su macroporosi Polymer Monoliti di avanzata Arricchimento fosfopeptidi

We describe a protocol for the preparation of hybrid materials based on highly porous coordination polymer coatings on the internal surface of macroporous ...

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next generation photosensitizers for Photodynamic Therapy (PDT) is reported. The nanoparticles are formed by hydrophobic interaction of the semiconducting polymer MEH-PPV (poly[2-methoxy-5-(2-ethylhexyloxy)-1,4-phenylenevinylene]) with the fullerene PCBM (phenyl-C61-butyric acid methyl ester) in the presence of a non-compatible solvent. MEH-PPV has a high extinction coefficient that leads to high rates of triplet formation, and efficient charge and energy transfer to the fullerene PCBM. The latter processes enhance the efficiency of the PDT system through fullerene assisted triplet and radical formation, and ultrafast deactivation of MEH-PPV excited stated. The results reported here show that this nanoparticle PDT sensitizing system is highly effective and shows unexpected specificity to cancer cell lines.

This protocol describes a method for the fabrication of conducting polymer nanoparticles blended with fullerene. These nanoparticles were investigated for their potential use as a next generation photosensitizers for Photodynamic Therapy (PDT).

Terapia fotodinamica con Blended Condurre Polimero / Fullerene nanoparticelle fotosensibilizzanti

In this article a method for the fabrication and reproducible in-vitro evaluation of conducting polymer nanoparticles blended with fullerene as the next ...

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

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

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

Raffreddamento Vota dipendenti Misure ellissometria per determinare la dinamica dei Thin Films Glassy

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

The Preparation and Properties of Thermo-reversibly Cross-linked Rubber Via Diels-Alder Chemistry

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ethylene-propylene rubber, grafted with maleic anhydride, is thermo-reversibly cross-linked in two steps. The pending anhydride moieties are first modified with furfurylamine to graft furan groups to the rubber backbone. These pendant furan groups are then cross-linked with a bis-maleimide via a Diels-Alder coupling reaction. Both reactions can be performed under a broad range of experimental conditions and can easily be applied on a large scale. The material properties of the resulting Diels-Alder cross-linked rubbers are similar to a peroxide-cured ethylene/propylene/diene rubber (EPDM) reference. The cross-links break at elevated temperatures (&#62; 150 &#176;C) via the retro-Diels-Alder reaction and can be reformed by thermal annealing at lower temperatures (50-70 &#176;C). Reversibility of the system was proven with infrared spectroscopy, solubility tests and mechanical properties. Recyclability of the material was also shown in a practical way, i.e., by cutting a cross-linked sample into small parts and compression molding them into new samples displaying comparable mechanical properties, which is not possible for conventionally cross-linked rubbers.

A simple two-step approach involving rubber modification and cross-linking yields fully reworkable, elastic rubber products.

La preparazione e la proprietà di Thermo-reversibile reticolato Chimica Gomma Via Diels-Alder

A method for using Diels Alder thermo-reversible chemistry as cross-linking tool for rubber products is demonstrated. In this work, a commercial ...

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

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

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

Elettroforesi capillare per monitorare Peptide innesto su Chitosano film in tempo reale

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

Fabrication and Testing of Photonic Thermometers

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

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

Fabbricazione e collaudo di termometri fotonici

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

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables the silk proteins to be compact and ordered by shearing and elongation forces. Here, a biomimetic microfluidic channel was designed to mimic the specific geometry of the spinning duct of the silkworm. Regenerated silk fibroin (RSF) spinning doped with high concentration, was extruded through the microchannel to dry-spin fibers at ambient temperature and pressure. In the post-treated process, the as-spun fibers were drawn and stored in ethanol aqueous solution. Synchrotron radiation wide-angle X-ray diffraction (SR-WAXD) technology was used to investigate the microstructure of single RSF fibers, which were fixed to a sample holder with the RSF fiber axis normal to the microbeam of the X-ray. The crystallinity, crystallite size, and crystalline orientation of the fiber were calculated from the WAXD data. The diffraction arcs near the equator of the two-dimensional WAXD pattern indicate that the post-treated RSF fiber has a high orientation degree.

A protocol for the microfluidic spinning and microstructure characterization of regenerated silk fibroin monofilament is presented.

A secco microfluidic-spinning e caratterizzazione delle fibre rigenerate seta Fibroin

The protocol demonstrates a method for mimicking the spinning process of silkworm. In the native spinning process, the contracting spinning duct enables ...

Time-resolved Photophysical Characterization of Triplet-harvesting Organic Compounds at an Oxygen-free Environment Using an iCCD Camera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables the acquisition of photoluminescence spectra covering the time regime from nanoseconds up to 0.1 s. This enables us to follow the changes in the intensity (decay) and emission of the spectra over time. Using this method, it is possible to study diverse photophysical phenomena, such as the emission of phosphorescence, and the contributions of prompt and delayed fluorescence in molecules showing thermally activated delayed fluorescence (TADF). Remarkably, all spectra and decays are obtained in a single experiment. This can be done for solids (thin film, powder, crystal) and liquid samples, where the only limitations are the spectral sensitivity of the camera and the excitation wavelength (532 nm, 355 nm, 337 nm, and 266 nm). This technique is, thus, very important when investigating the excited state dynamics in organic emitters for their application in organic light-emitting diodes and other areas where triplet harvesting is of paramount importance. Since triplet states are strongly quenched by oxygen, emitters with efficient TADF luminescence, or those showing room temperature phosphorescence (RTP), must be correctly prepared in order to remove any dissolved oxygen from solutions and films. Otherwise, no long-lived emission will be observed. The method of degassing solid samples as presented in this work is basic and simple, but the degassing of liquid samples creates additional difficulties and is particularly interesting. A method of minimizing solvent loss and changing the sample concentration, while still enabling to remove oxygen in a very efficient and a repeatable manner, is presented in this work.

Here, we present a method of the spectroscopic characterization of organic molecules by means of time-resolved photoluminescence spectroscopy on the nanosecond-to-millisecond timescale in oxygen-free conditions. Methods to efficiently remove oxygen from the samples and, thus, limit luminescence quenching are also described.

Tempo-risolta caratterizzazione fotofisica di tripletto-raccoglitrici composti organici a un utilizzo di ambiente privo di ossigeno un iCCD telecamera

Here, we present a sensible method of the acquisition and analysis of time-resolved photoluminescence using an ultrafast iCCD camera. This system enables ...