Este trabajo fue financiado en parte por el Fondo de Texas Emerging Technology (inicio a la tuberculosis), el Programa de Mejora de Texas State University Research, el Texas State University Doctorado Becas de Investigación (al TC), la Asociación de la NSF para la Investigación y Educación en Materiales (PREM, DMR-1205670), la Fundación Welch (AI-0045), y los Institutos Nacionales de Salud (R01CA032132).

<ol>
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The authors have nothing to disclose.

En este trabajo, los PN de polímeros electroactivos se han sintetizado como agentes potenciales de PTT para el tratamiento del cáncer. La preparación de los NPs se describe, a partir de la síntesis de los monómeros seguido por polimerización en emulsión. Mientras que la preparación de NPs utilizando polímeros electroactivos tales como EDOT y pirrol se ha descrito antes, este documento describe la preparación de NPs poliméricos a partir de monómeros de conjugación extendidos únicos, lo que demuestra que est...

Polímeros electroactivos cambian sus propiedades (color, conductividad, reactividad, volumen, etc.) en presencia de un campo eléctrico. Los tiempos de conmutación rápidos, tunability, la durabilidad, y las características de peso ligero de polímeros electroactivos han dado lugar a muchas aplicaciones propuestas, incluida la energía alternativa, sensores, Electrochromics, y dispositivos biomédicos. Polímeros electroactivos son potencialmente útiles como, baterías y condensadores electrodos ligeros flexibles. 1 Aplicaciones de polímeros electroactivos en dispositivos electrocrómicos incluyen sistemas de reducción de deslumbramiento para edificios y automóviles, gafas de sol, gafas de protección, dispositivos de almacenamiento ópticos y textiles inteligentes. 2.5 ventanas inteligentes pueden reducir los requerimientos de energía mediante el bloqueo de determinadas longitudes de onda de la luz a la carta y la protección de los interiores de las casas y automóviles. Textiles inteligentes pueden ser utilizados en la ropa para ayudar a proteger contra la radiación UV. 6 polímeros electroactivos tienen als,o comenzado a ser utilizado en dispositivos médicos. Entre los polímeros electroactivos utilizados en dispositivos biomédicos, polipirrol (PPy), polianilina (PANI), y poli (3,4-etilenodioxitiofeno) (PEDOT) se encuentran entre los más comunes. Por ejemplo, estos tipos de polímeros se utilizan comúnmente como transductores en dispositivos biosensores 7 Aplicaciones en la entrega terapéutico también se han mostrado prometedores.; estudios han demostrado la liberación de los fármacos y proteínas terapéuticas de los dispositivos preparados a partir de polímeros electroactivos 8-12. Más recientemente, polímeros electroactivos se han utilizado como agentes terapéuticos en la terapia fototérmica 13-15. En la terapia fototérmica, agentes fototérmicos deben absorber la luz en el Cercano infrarrojo de (NIR) región (~ de 700-900 nm), también conocida como la ventana terapéutica, donde la luz tiene la profundidad máxima de penetración en el tejido, típicamente de hasta 1 cm. 16,17 En este rango, cromóforos biológicos tales como la hemoglobina , la hemoglobina oxigenada, lípidos y agua tienen poco que-noabsorbancia, que permite que la luz penetre fácilmente. Cuando los agentes fototérmicos absorben la luz en esta ventana terapéutica, la foto energético se convierte en energía fototérmica. Irvin y colaboradores han informado anteriormente alcoxi-monómeros sustituidos de benceno bis-Edot que se sintetizaron usando un acoplamiento de Negishi. 18 de acoplamiento de Negishi es un método preferido para la formación de enlaces carbono-carbono. Este proceso tiene muchas ventajas, incluyendo el uso de productos intermedios organometálicos de cinc, que son menos tóxicos y tienden a tener mayor reactividad que otros compuestos organometálicos utilizados. 19,20 compuestos orgánico de zinc también son compatibles con una amplia gama de grupos funcionales en los organohaluros. 20 En el reacción de acoplamiento de Negishi, un organohaluro y organometálico están acoplados mediante el uso de un catalizador de paladio (0) catalizador. 20 En el trabajo presentado en el presente documento, este método de acoplamiento cruzado se utiliza en la síntesis de 1,4-dialcoxi-2,5-bis ( 3,4-ethylenedioxythienyl) benzemonómeros ne (2 Bedot-B (OR)). Estos monómeros pueden ser fácilmente polimerizan electroquímicamente o químicamente para producir polímeros que son candidatos prometedores para su uso en aplicaciones biomédicas. Los métodos convencionales para la preparación de suspensiones poliméricas coloidales en soluciones acuosas para aplicaciones biomédicas implican típicamente la disolución de polímeros a granel seguido por nanoprecipitation o emulsión técnicas de evaporación de disolvente. 21,22 A fin de producir NPs de poli (Bedot-B (OR) 2) , un enfoque de abajo hacia arriba se demuestra aquí, donde los PN se sintetizan a través de polimerización en emulsión situ. La polimerización en emulsión es un proceso que es fácilmente escalable y es un método relativamente rápido para la preparación de NP. 22 Los estudios que utilizan la polimerización en emulsión para producir NPs de otros polímeros electroactivos se han reportado para PPy y PEDOT. 15,23,24 PEDOT NPs, por ejemplo, se han preparado utilizando emulsión de aerosol polymerization. 24 Este método es difícil de reproducir, y por lo general produce, partículas de tamaño micrométrico más grandes. El protocolo se describe en este artículo explora el uso de un método de la gota-sonicación para preparar de forma reproducible 100 nm PN polímero. En este protocolo, los polímeros electroactivos adaptados para absorber la luz en la región NIR similar al poli informó anteriormente (Bedot-B (OR) 2) se sintetizan y caracterizado para demostrar su potencial en dispositivos electrocrómicos y como agentes de PTT. En primer lugar, se describe el protocolo para la síntesis de los monómeros a través de acoplamiento de Negishi. Los monómeros se caracterizan usando espectroscopía de RMN y UV-Vis-NIR. También se describe la preparación de suspensiones coloidales NP a través de polimerización en emulsión oxidativo en medios acuosos. El procedimiento se basa en un proceso de polimerización en emulsión de dos etapas descrito previamente por Han et al. Que se aplica a los diferentes monómeros. Un sistema de dos tensioactivo esutilizado para controlar el monodispersidad NP. Un ensayo de viabilidad celular se utiliza para evaluar citocompatibilidad de los NPs. Por último, el potencial de estas NPs para actuar como transductores de PTT se demuestra por la irradiación con un láser NIR.

<table border="0" cellpadding="0" cellspacing="0" width="747">
	<tbody>
		<tr height="42">
			<td height="42" style="height:42px;width:291px;">2 mm diameter platinum working electrode</td>
			<td style="width:171px;">CH Instruments</td>
			<td style="width:119px;">CH102</td>
			<td style="width:167px;">Polished using very fine sandpaper</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:291px;">3,4-ethylenedioxythiophene</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">483028</td>
			<td style="width:167px;">Purified by vacuum distillation</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:291px;">3-(4,5-Dimethylthiazol-2-yl)-2,5-Diphenyltetrazolium Bromide (MTT) 98%</td>
			<td>Alfa Aesar</td>
			<td style="width:119px;">L11939</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">505 Sonic Dismembrator</td>
			<td>Fisher Scientific&#8482;&#160;</td>
			<td style="width:119px;">FB505110</td>
			<td style="width:167px;">1/8 &#8220; tip and rated at 500 watts</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">808 nm laser diode</td>
			<td>ThorLabs</td>
			<td style="width:119px;">L808P1WJ</td>
			<td style="width:167px;">Rated at 1 W</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Acetonitrile anhydrous 99%</td>
			<td>Acros</td>
			<td style="width:119px;">61022-0010</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Avanti J-26 XPI</td>
			<td>Beckman Coulter</td>
			<td style="width:119px;">393127</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Bromohexane 98%</td>
			<td>MP Biomedicals</td>
			<td style="width:119px;">202323</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Dialysis (100,000) MWCO</td>
			<td>SpectrumLabs</td>
			<td style="width:119px;">G235071</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Dimethyl sulfoxide 99% (DMSO)</td>
			<td>BDH</td>
			<td style="width:119px;">BDH1115</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Dimethylformamide anhydrous (DMF) 99%</td>
			<td>Acros</td>
			<td style="width:119px;">326870010</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Dodecyl benzenesulfonate (DBSA)&#160;</td>
			<td>TCI</td>
			<td style="width:119px;">D0989</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Dulbecco&#8217;s modified eagle medium (DMEM)&#160;</td>
			<td>Corning</td>
			<td style="width:119px;">10-013 CV</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;">EMS 150 TES sputter coater</td>
			<td style="width:171px;">Electron Microscopy Sciences</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Ethanol (EtOH) 100%</td>
			<td>BDH</td>
			<td style="width:119px;">BDH1156</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">ethyl 4-bromobutyrate (98%)</td>
			<td>Acros</td>
			<td style="width:119px;">173551000</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Ethyl acetate 99%</td>
			<td>Fisher</td>
			<td style="width:119px;">UN1173</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">Fetal bovine serum (FBS)</td>
			<td>Corning</td>
			<td style="width:119px;">35-010-CV</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Helios NanoLab 400</td>
			<td>FEI</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Hexane</td>
			<td>Fisher</td>
			<td style="width:119px;">H306-4</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Hydrochloric acid (HCl)</td>
			<td>Fisher</td>
			<td style="width:119px;">A142-212</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Hydroquinone 99.5%</td>
			<td>Acros</td>
			<td style="width:119px;">120915000</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Hydrozine anhydrous 98%</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">215155</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Indium tin oxide (ITO) coated galss</td>
			<td>Delta Technologies</td>
			<td style="width:119px;">CG-41IN-CUV</td>
			<td style="width:167px;">4-8 &#937;/sq</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:291px;">Iron chloride 97% FeCl3</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">157740</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:291px;">Magnesium sulfate (MgSO4)</td>
			<td>Fisher</td>
			<td style="width:119px;">593295</td>
			<td style="width:167px;">Dried at 100 oC</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">SKOV-3</td>
			<td>ATCC</td>
			<td style="width:119px;">HTB-26</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Methanol</td>
			<td>BDH</td>
			<td style="width:119px;">BHD1135</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">n-Butlithium (2.5 M)&#160;</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">230707</td>
			<td style="width:167px;">Pyrophoric</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:291px;">Poly(styrenesulfonate-co-malic acid) (PSS-co-MA) 20,000 MW</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">434566</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:291px;">Potassium carbonate</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">209619</td>
			<td style="width:167px;">Dried at 100 oC</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Potassium hydroxide</td>
			<td>Alfa Aesar</td>
			<td style="width:119px;">A18854</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Potassium iodide</td>
			<td>Fisher</td>
			<td style="width:119px;">P410-100</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">RO-5 stirplate</td>
			<td>IKA-Werke</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">SC4000 IR camera</td>
			<td>FLIR</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Synergy H4 Hybrid Reader</td>
			<td>Biotek</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:291px;">Tetrabutylammonium perchlorate (TBAP) 99%</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">3579274</td>
			<td style="width:167px;">Purified by recrystallization in ethyl acetate</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Tetrahydrofuran anhydrous (THF) 99%</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">401757</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">tetrakis(triphenylphosphine) 
			palladium(0)</td>
			<td>Sigma-Aldrich</td>
			<td style="width:119px;">216666</td>
			<td style="width:167px;">Moisture sensitive</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">Thermomixer</td>
			<td>Eppendorf</td>
			<td style="width:119px;"></td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;width:291px;">USB potentiostat/galvanostat</td>
			<td>WaveNow</td>
			<td style="width:119px;">AFTP1</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:291px;">Zetasizer Nano Zs</td>
			<td>Malvern</td>
			<td style="width:119px;"></td>
			<td style="width:167px;">Optical Arrangment 175o</td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;width:291px;">Zinc chloride (1 M) ZnCl2</td>
			<td>Acros</td>
			<td style="width:119px;">370057000</td>
			<td style="width:167px;"></td>
		</tr>
	</tbody>
</table>

electroactive polymer nanoparticles exhibiting photothermal properties

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

El protocolo de reacción produciendo M1 y M2 se muestra en la Figura 1. Los monómeros se pueden caracterizar por 1 H y 13 C RMN espectroscopía, punto de fusión, y análisis elemental. El espectro de RMN 1H proporciona información sobre la conectividad de los átomos y sus entornos electrónicos; por lo tanto, se utiliza de manera rutinaria para verificar que las reacciones se han completado con éxito. Reacciones de ...

Watch this Scientific Journal Video about Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties at JoVE.com

Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

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

Propiedades Electroactivos Polymer Nanopartículas Exponer fototérmica

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

electroactive-polymer-nanoparticles-exhibiting-photothermal-properties

Research

JoVE Journal

Engineering

13.7K vistas.  Texas State University. A protocol is presented for the synthesis and preparation of nanoparticles consisting of electroactive polymers. 

Video: Electroactive Polymer Nanoparticles Exhibiting Photothermal Properties

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 litografía para la generación de microempresas y patrones de submicrónicas de sustratos poliméricos

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

Investigación

Ingeniería

Optical Trapping of Nanoparticles

Optical trapping is a technique for immobilizing and manipulating small objects in a gentle way using light, and it has been widely applied in trapping and manipulating small biological particles. Ashkin and co-workers first demonstrated optical tweezers using a single focused beam1. The single beam trap can be described accurately using the perturbative gradient force formulation in the case of small Rayleigh regime particles1. In the perturbative regime, the optical power required for trapping a particle scales as the inverse fourth power of the particle size. High optical powers can damage dielectric particles and cause heating. For instance, trapped latex spheres of 109 nm in diameter were destroyed by a 15 mW beam in 25 sec1, which has serious implications for biological matter2,3.
A self-induced back-action (SIBA) optical trapping was proposed to trap 50 nm polystyrene spheres in the non-perturbative regime4. In a non-perturbative regime, even a small particle with little permittivity contrast to the background can influence significantly the ambient electromagnetic field and induce a large optical force. As a particle enters an illuminated aperture, light transmission increases dramatically because of dielectric loading. If the particle attempts to leave the aperture, decreased transmission causes a change in momentum outwards from the hole and, by Newton's Third Law, results in a force on the particle inwards into the hole, trapping the particle. The light transmission can be monitored; hence, the trap can become a sensor. The SIBA trapping technique can be further improved by using a double-nanohole structure.
The double-nanohole structure has been shown to give a strong local field enhancement5,6. Between the two sharp tips of the double-nanohole, a small particle can cause a large change in optical transmission, thereby inducing a large optical force. As a result, smaller nanoparticles can be trapped, such as 12 nm silicate spheres7 and 3.4 nm hydrodynamic radius bovine serum albumin proteins8. In this work, the experimental configuration used for nanoparticle trapping is outlined. First, we detail the assembly of the trapping setup which is based on a Thorlabs Optical Tweezer Kit. Next, we explain the nanofabrication procedure of the double-nanohole in a metal film, the fabrication of the microfluidic chamber and the sample preparation. Finally, we detail the data acquisition procedure and provide typical results for trapping 20 nm polystyrene nanospheres.

The following setup approach details low power optical trapping of dielectric nanoparticles using a double-nanohole in metal film.

Trampas ópticas de las nanopartículas

Optical trapping is a technique for immobilizing and manipulating small objects in a gentle way using light, and it has been widely applied in trapping ...

Preparation and Friction Force Microscopy Measurements of Immiscible, Opposing Polymer Brushes

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low friction at the interface. Nevertheless, these systems can be sensitive to wear due to interdigitation of the opposing brushes. In a recent publication, we have shown via molecular dynamics simulations and atomic force microscopy experiments, that using an immiscible polymer brush system terminating the substrate and the slider surfaces, respectively, can eliminate such interdigitation. As a consequence, wear in the contacts is reduced. Moreover, the friction force is two orders of magnitude lower compared to traditional miscible polymer brush systems. This newly proposed system therefore holds great potential for application in industry. Here, the methodology to construct an immiscible polymer brush system of two different brushes each solvated by their own preferred solvent is presented. The procedure how to graft poly(N-isopropylacrylamide) (PNIPAM) from a flat surface and poly(methyl methacrylate) (PMMA) from an atomic force microscopy (AFM) colloidal probe is described. PNIPAM is solvated in water and PMMA in acetophenone. Via friction force AFM measurements, it is shown that the friction for this system is indeed reduced by two orders of magnitude compared to the miscible system of PMMA on PMMA solvated in acetophenone.

The methodology to perform friction force microscopy experiments for contacting brushes is presented: Two polymer brushes that are grafted from (a) substrates and (b) colloidal probes are slid to show that, by using two contacting immiscible brush systems, friction in sliding contacts is reduced compared to miscible brush systems.

Preparación y Fricción Fuerza Microscopía mediciones de inmiscibles, opuestos polímero Cepillos

Solvated polymer brushes are well known to lubricate high-pressure contacts, because they can sustain a positive normal load while maintaining low ...

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to neutral gold Au(0) by reducing agents, such as sodium citrate or sodium borohydride. The extension of this method to decorate iron oxide or similar nanoparticles with gold nanoparticles to create multifunctional hybrid Fe2O3-Au nanoparticles is straightforward. This approach yields fairly good control over Au nanoparticle dimensions and loading onto Fe2O3. Additionally, the Au metal size, shape, and loading can easily be tuned by changing experimental parameters (e.g., reactant concentrations, reducing agents, surfactants, etc.). An advantage of this procedure is that the reaction can be done in air or water, and, in principle, is amenable to scaling up. The use of such optically tunable Fe2O3-Au nanoparticles for hyperthermia studies is an attractive option as it capitalizes on plasmonic heating of gold nanoparticles tuned to absorb light strongly in the VIS-NIR region. In addition to its plasmonic effects, nanoscale Au provides a unique surface for interesting chemistries and catalysis. The Fe2O3 material provides additional functionality due to its magnetic property. For example, an external magnetic field could be used to collect and recycle the hybrid Fe2O3-Au nanoparticles after a catalytic experiment, or alternatively, the magnetic Fe2O3 can be used for hyperthermia studies through magnetic heat induction. The photothermal experiment described in this report measures bulk temperature change and nanoparticle solution mass loss as functions of time using infrared thermocouples and a balance, respectively. The ease of sample preparation and the use of readily available equipment are distinct advantages of this technique. A caveat is that these photothermal measurements assess the bulk solution temperature and not the surface of the nanoparticle where the heat is transduced and the temperature is likely to be higher.

Multifunctional Hybrid Fe2O3-Au Nanoparticles for Efficient Plasmonic Heating

We describe the synthesis and properties of multifunctional Fe2O3-Au nanoparticles produced by a wet chemical approach and investigate their photothermal properties using laser irradiation. The composite Fe2O3-Au nanoparticles retain the properties of both materials, creating a multifunctional structure with excellent magnetic and plasmonic properties.

Multifuncional híbrido Fe<sub&gt; 2</sub&gt; O<sub&gt; 3</sub&gt; -Au Nanopartículas para la calefacción eficiente plasmónicas

One of the most widely used methods for manufacturing colloidal gold nanospherical particles involves the reduction of chloroauric acid (HAuCl4) to ...

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices have used devices prepared by spin coating, a process that is not amenable to large-scale fabrication. This mismatch in device fabrication makes it difficult to translate quantitative results obtained in the laboratory to the commercial level, making optimization difficult. Using a mini-slot die coater, this mismatch can be resolved by translating the commercial process to the laboratory and characterizing the structure formation in the active layer of the device in real time and in situ as films are coated onto a substrate. The evolution of the morphology was characterized under different conditions, allowing us to propose a mechanism by which the structures form and grow. This mini-slot die coater offers a simple, convenient, material efficient route by which the morphology in the active layer can be optimized under industrially relevant conditions. The goal of this protocol is to show experimental details of how a solar cell device is fabricated using a mini-slot die coater and technical details of running in situ structure characterization using the mini-slot die coater.

Printing Fabrication of Bulk Heterojunction Solar Cells and In Situ Morphology Characterization

Here, we present a protocol to fabricate organic thin film solar cells using a mini-slot die coater and related in-line structure characterizations using synchrotron scattering techniques.

La fabricación de la impresión a granel heterounión células solares y<em&gt; In Situ</em&gt; Morfología Caracterización

Polymer-based materials hold promise as low-cost, flexible efficient photovoltaic devices. Most laboratory efforts to achieve high performance devices ...

Advanced Compositional Analysis of Nanoparticle-polymer Composites Using Direct Fluorescence Imaging

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise composition of these materials is essential, especially in the design of surface catalysts, where the surface concentration of the active component determines the activity of the material. Antimicrobial materials which utilize nanoparticles are a particular focus of this technology. Recently swell encapsulation has emerged as a technique for inserting antimicrobial nanoparticles into a host polymer matrix. Swell encapsulation provides the advantage of localizing the incorporation to the external surfaces of materials, which act as the active sites of these materials. However, quantification of this nanoparticle uptake is challenging. Previous studies explore the link between antimicrobial activity and surface concentration of the active component, but this is not directly visualized. Here we show a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of CdSe/ZnS nanoparticles can be accurately visualized through cross-sectional fluorescence imaging. Using this method, we can quantify the uptake of nanoparticles via swell encapsulation and measure the surface concentration of encapsulated particles, which is key in optimizing the activity of functional materials.

Here we present a reliable method to monitor the incorporation of nanoparticles into a polymer host matrix via swell encapsulation. We show that the surface concentration of cadmium selenide quantum dots can be accurately visualized through cross-sectional fluorescence imaging.

Análisis de la composición avanzada de compuestos de nanopartículas poliméricas Uso de la imagen de fluorescencia directa

The fabrication of polymer-nanoparticle composites is extremely important in the development of many functional materials. Identifying the precise ...

Inkjet-printed Polyvinyl Alcohol Multilayers

Inkjet printing is a modern method for polymer processing, and in this work, we demonstrate that this technology is capable of producing polyvinyl alcohol (PVOH) multilayer structures. A polyvinyl alcohol aqueous solution was formulated. The intrinsic properties of the ink, such as surface tension, viscosity, pH, and time stability, were investigated. The PVOH-based ink was a neutral solution (pH 6.7) with a surface tension of 39.3 mN/m and a viscosity of 7.5 cP. The ink displayed pseudoplastic (non-Newtonian shear thinning) behavior at low shear rates, and overall, it demonstrated good time stability. The wettability of the ink on different substrates was investigated, and glass was identified as the most suitable substrate in this particular case. A proprietary 3D inkjet printer was employed to manufacture polymer multilayer structures. The morphology, surface profile, and thickness uniformity of inkjet-printed multilayers were evaluated via optical microscopy.

An inkjet printer was used to manufacture polyvinyl alcohol multilayers. Polyvinyl alcohol water-based ink was formulated, and the main physical properties were investigated.

Multilingüe de alcohol polivinílico impreso con chorro de tinta

Inkjet printing is a modern method for polymer processing, and in this work, we demonstrate that this technology is capable of producing polyvinyl alcohol ...

Subsurface Defect Localization by Structured Heating Using Laser Projected Photothermal Thermography

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering thermal wave fields that are disturbed by the defect. This effect is measured and used to locate the defect. We form the destructively interfering wave fields by using a modified projector. The original light engine of the projector is replaced with a fiber-coupled high-power diode laser. Its beam is shaped and aligned to the projector&#39;s spatial light modulator and optimized for optimal optical throughput and homogeneous projection by first characterizing the beam profile, and, second, correcting it mechanically and numerically. A high-performance infrared (IR) camera is set up according to the tight geometrical situation (including corrections of the geometrical image distortions) and the requirement to detect weak temperature oscillations at the sample surface. Data acquisition can be performed once a synchronization between the individual thermal wave field sources, the scanning stage, and the IR camera is established by using a dedicated experimental setup which needs to be tuned to the specific material being investigated. During data post-processing, the relevant information on the presence of a defect below the surface of the sample is extracted. It is retrieved from the oscillating part of the acquired thermal radiation coming from the so-called depletion line of the sample surface. The exact location of the defect is deduced from the analysis of the spatial-temporal shape of these oscillations in a final step. The method is reference-free and very sensitive to changes within the thermal wave field. So far, the method has been tested with steel samples but is applicable to different materials as well, in particular to temperature sensitive materials.

This method aims at locating vertical subsurface defects. Here, we couple a laser with a spatial light modulator and trigger its video input to heat a sample surface deterministically with two anti-phased modulated lines while acquiring highly resolved thermal images. The defect position is retrieved from evaluating thermal wave interference minima.

Localización del defecto subsuperficial mediante calentamiento estructurado mediante termografía fototérmica proyectada con láser

The presented method is used to locate subsurface defects oriented perpendicularly to the surface. To achieve this, we create destructively interfering ...

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, interface precipitation, and mini-emulsion. In all methods, well-defined, micrometer-sized spheres are obtained from a self-assembling process in solution. The vapor diffusion method can result in spheres with the highest sphericity and surface smoothness, yet the types of the polymers able to form these spheres are limited. On the other hand, in the mini-emulsion method, microspheres can be made from various types of polymers, even from highly crystalline polymers with coplanar, &#960;-conjugated backbones. The photoluminescent (PL) properties from single isolated microspheres are unusual: the PL is confined inside the spheres, propagates at the circumference of the spheres via the total internal reflection at the polymer/air interface, and self-interferes to show sharp and periodic resonant PL lines. These resonating modes are so-called "whispering gallery modes" (WGMs). This work demonstrates how to measure WGM PL from single isolated spheres using the micro-photoluminescence (&#181;-PL) technique. In this technique, a focused laser beam irradiates a single microsphere, and the luminescence is detected by a spectrometer. A micromanipulation technique is then used to connect the microspheres one by one and to demonstrate the intersphere PL propagation and color conversion from coupled microspheres upon excitation at the perimeter of one sphere and detection of PL from the other microsphere. These techniques, &#181;-PL and micromanipulation, are useful for experiments on micro-optic application using polymer materials.

Protocols for the synthesis of microspheres from polymers, the manipulation of microspheres, and micro-photoluminescence measurements are presented.

Fabricación de microesferas de polímero para aplicaciones de resonador óptico y láser

This paper describes three methods of preparing fluorescent microspheres comprising &#960;-conjugated or non-conjugated polymers: vapor diffusion, ...

Production and Characterization of Vacuum Deposited Organic Light Emitting Diodes

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex donor-acceptor emitters is presented. With a step-by-step procedure, readers will be able to repeat and produce OLED devices based on simple organic emitters. A patterning procedure allowing the creation of personalized indium tin oxide (ITO) shape is shown. This is followed by the evaporation of all layers, encapsulation and characterization of each individual device. The end goal is to present a procedure that will give the opportunity to repeat the information presented in cited publication but also using different compounds and structures in order to prepare efficient OLEDs.

A protocol for the production of simple structured organic light-emitting diodes (OLEDs) is presented.

Producción y caracterización de vacío depositan diodos electroluminosos orgánicos

A method for producing simple and efficient thermally-activated delayed fluorescence organic light-emitting diodes (OLEDs) based on guest-host or exciplex ...