Este trabajo fue parcialmente apoyado por KAKENHI (25708020, 15K13812, 15H00860, 15H00986, 16H02081) de JSPS / MEXT Japón, la Asahi Glass Foundation y la Universidad de Tsukuba Pre-estratégica iniciativa, &quot;Conjunto de luz con asuntos y vida&quot;.

1. Protocolos de Fabricación de Microsferas de Polímero <ol><li> Método de Difusión de Vapor <ol><li> Se disuelven 2 mg de polímeros conjugados, tales como P1 (poli [(9,9 - dioctilfluoreno - 2,7 - diil) - alt - (5 - octiltieno [3,4 - c ] pirrol - 4,6 - diona - 1, 3 - diil)]) 28 y P2 (poli [(N- (2 - heptilundecyl) carbazol - 2,7 - diil) - alt - (4,8 - bis [(dodecil) carbonil] benzo [1,2b] : 4,5- b &#39;] ditiofeno-2,6-diil)]) 28 , en 2 ml de cloroformo (un buen disolvente) en un vial de 5 ml. </li><li> Ponga 5 ml de metanol (un disolvente pobre) en un vial de 50 ml. </li><li> Colocar el vial de 5 ml que contiene la solución de cloroformo del polímero en el vial de 50 ml que contiene metanol. </li><li> Se tapa el vial de 50 ml y se mantiene durante 3 días a 25 ° C para permitir la precipitación de las microesferas de polímero. </li></ol></li><li> Método de la mini-emulsión <ol><li> Disolver 5 mg de polímeros conjugados, tales como polY [9,9-di-n-octilfluorenil-2,7-diil] (PFO) y poli [2-metoxi-5- (3 &#39;, 7&#39;-dimetiloctiloxi) -1,4-fenilenvinileno] (MDMOPPV) En 1 ml de cloroformo. </li><li> Disolver 30 mg (~ 50 mM) de dodecilsulfato sódico (SDS) en 2 mL de agua desionizada. </li><li> Añadir 100 μl de la solución de cloroformo del polímero a 2 ml de agua que contiene SDS. </li><li> Agitar vigorosamente la mezcla de cloroformo / agua usando un homogeneizador de ultra alta velocidad a 30.000 rpm durante 2 minutos para emulsionar la solución. </li><li> Manténgalo durante 1 día sin tapar el vial para evaporar el cloroformo. </li><li> Centrifugar la dispersión en un tubo de microcentrífuga de 1,5 ml durante 5 min a 2,200 x g. Eliminar la solución acuosa sobrenadante que contiene SDS. </li><li> Añadir 2 ml de agua desionizada y agitar vigorosamente. </li><li> Repita los pasos 1.2.6 y 1.2.7 tres veces para lavar el SDS residual. </li></ol></li><li> Método de precipitación de la interfaz </li><li> Disolver 200 μg de poliestireno (PS) y 10 μG de colorante fluorescente (borir dipirina, BODIPY) a 0,2 ml de tetrahidrofurano (THF). </li><li> Verter suavemente la solución de THF en 1 mL de la capa de agua. </li><li> Mantenga el THF / agua separado de dos capas durante 6 h sin tapar el vial para permitir la precipitación de las microesferas de polímero. </li></ol> 2. Micro-fotoluminiscencia (μ-PL) Medición <ol><li> Preparación de la muestra <ol><li> Diluir una suspensión de las microesferas preparadas en la sección 1 en un no disolvente ( es decir, metanol o agua desionizada). </li><li> Se centrifuga una gota (20-30 μl) de la suspensión diluida de las microesferas sobre un substrato de cuarzo usando un recubridor por centrifugación (típicamente, 2000 rpm durante 50 s). </li><li> Secar al aire la película moldeada resultante hasta que los disolventes se hayan evaporado completamente (~ 5 min). </li></ol></li><li> Configuración experimental <ol><li> Poner el sustrato de cuarzo (15 x 15 x 0,5 mm 3 ) en la etapa de muestra de un micrófono ópticoOscope </li><li> Encuentre microesferas bien definidas que estén aisladas de otras esferas y apropiadas para la medición μ-PL. </li><li> Seleccione un láser ( es decir, longitud de onda, onda continua o pulso, tiempo de irradiación, integración, etc. ). </li><li> Seleccione la ampliación de la lente. </li></ol></li><li> Mediciones <ol><li> Utilice un rayo láser enfocado para irradiar la microesfera. Utilice la siguiente condición láser: cw o láser pulsado con longitudes de onda de excitación ( λ ex ) de 405 nm (cw), 450 nm (cw), 355 nm (láser de pulso, frecuencia, 1 kHz, duración del impulso, 7 ns) y 470 Nm (pulso láser, frecuencia, 2,5 MHz, duración del impulso, 70 ps). </li><li> Registre el espectro PL en el punto excitado utilizando un espectrómetro con una rejilla de 300 o 1.200 ranuras mm -1 . </li><li> Tome una imagen fluorescente. </li><li> Cambie el punto de excitación moviendo la etapa de muestra. </li><li> Cambiar el punto de detección inclinando el colimador(si necesario). </li></ol></li></ol> 3. Técnica de Micromanipulación <ol><li> Manipulación de microesferas <ol><li> Establecer un sustrato de cuarzo sobre el que las microesferas se inmovilizan en la etapa de la muestra de un microscopio óptico. </li><li> Encuentre una microesfera bien definida apropiada para la medición μ-PL. </li><li> Coloque una microaguja de plástico en un aparato de micro-manipulación. </li><li> Mueva la micro-aguja con un joystick controlado por computadora para recoger una microesfera. </li><li> Mueva la microesfera y conéctela a otra microesfera. </li><li> Mida el μ-PL de la microesfera conectada. </li></ol></li></ol>

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Los autores declaran que no hay intereses financieros en competencia.

The selection of a good solvent and non-solvent is very important for the self-assembly of well-defined microspheres. If the solubility of a polymer is too high, precipitation will not occur. Also, in general, &#960;-conjugated polymers are hydrophobic, so polar non-solvents, such as MeOH, acetonitrile, and acetone, are often used in the vapor diffusion method to minimize the surface energy required to form a spherical shape. The interface precipitation method is often adopted for the preparation of dye-doped polymer microspheres. Non-conjugated polymers, such as polystyrene, poly(methylmethacrylate), and poly(dimethylsiloxane), are often used as the sphere medium. These polymers are less hydrophobic than typical &#960;-conjugated polymers, so heavy agglomeration does not occur after precipitation in water. If microspheres are not obtained using these methods, other methods, such as post-polymerization dispersion and emulsion polymerization, can be adopted33.
The crystallinity of polymers is the important factor. Generally, &#960;-conjugated polymers have a flat, &#960;-electronic plane. Thus, &#960;-stacking results in the crystallization of the polymers, which prevents the isotropic growth of spheres. Hence, polymers with highly twisted &#960;-electronic planes are favorable for the formation of well-defined microspheres, which prevents interchain &#960;-stacking and amorphous aggregation. To prepare microspheres from polymers with high crystallinity, the mini-emulsion method is appropriate. However, for this method, the surface morphology of the resultant spheres is not very smooth because of the coverage of the surfactant. 
The preferred method of observing WGM PL is to use a focused laser beam to irradiate the rim of a microsphere. The contact point with the substrate causes a defect in the microsphere where the confined light leaks. Therefore, when a focused laser is used to irradiate a microsphere, all the confined light passes through the contact point with the substrate. On the other hand, when the rim of the microsphere is excited, most routes of the confined light do not pass through the contact point with the substrate, leading to better confinement. Thus, well-defined, high-Q WGM PL lines appear.
To conduct WGM lasing from conjugated polymer microspheres, several conditions are required: [1] For the population inversion, high-density optical pumping is needed by using, for example, a femto-second laser pulse. [2] Polymers must hardly be photodamaged upon strong photoexcitation. [3] Highly dispersed microspheres with smooth surfaces are preferred. If these conditions are satisfied, WGM lasing properties can be observed from conjugated polymer microsphere resonators. Fluorescent dye-doped polymer microspheres are also applicable to chemical and biological sensing tools and can be used for laser and optical circuit applications34,35.

Las partículas de nano / micro dimensiones de polímero se usan ampliamente para una variedad de aplicaciones, incluyendo como soporte de catalizador, cargas de cromatografía en columna, agentes de liberación de fármacos, sondas fluorescentes para seguimiento de células, medios ópticos, etcétera 1 , 2 , 3 , 4 , 5 , 6 , 7 , 8 , 9 . En particular, los polímeros conjugados con π tienen propiedades luminescentes inherentes y propiedades de conducción de carga que son beneficiosas para aplicaciones ópticas, electrónicas y optoelectrónicas que utilizan esferas de polímero 10 , 11 , 12 , 13 , 14 , especialmente aplicaciones de láser que usan soft orgAnic materials 15 , 16 , 17 . Por ejemplo, la integración tridimensional de esferas con varios cientos de diámetros de nanómetro forma cristales coloidales, que muestran holguras de bandas fotónicas a una cierta longitud de onda 18 , 19 . Cuando la luz está confinada en la estructura periódica de la intersfera, la acción láser aparece en el centro de la banda de parada. Por otra parte, cuando el tamaño de las esferas aumenta a la escala de varios micrómetros, la luz se confina dentro de una sola microesfera a través de la reflexión interna total en la interfaz polımero / aire 20 . La propagación de la onda luminosa en la circunferencia máxima resulta en interferencia, dando lugar a la aparición de un modo resonante con líneas de emisión agudas y periódicas. Estos modos ópticos son los llamados &quot;modos de galería susurrantes&quot; (WGMs). El término &quot;galería susurrante&quot; se originóSt. Paul&#39;s Cathedral en Londres, donde las ondas sonoras se propagan a lo largo de la circunferencia de la pared, permitiendo susurros ser escuchado por una persona en el otro lado de la galería. Debido a que la longitud de onda de la luz está en la escala sub-micrométrica, que es mucho más pequeña que las ondas sonoras, una cúpula tan grande no es necesaria para el WGM de la luz: vasos diminutos, micrométricos, bien definidos, como microesferas, microdiscos , Y los microcristales, cumplen las condiciones de WGM. La ecuación 1 es una forma simple de la condición de resonancia WGM 21 : Nπd = lλ (1) Donde n es el índice de refracción del resonador, d es el diámetro, l es el número entero y λ es la longitud de onda de la luz. La parte izquierda de (1) es la longitud de la trayectoria óptica a través de una propagación de un círculo. Cuando la trayectoria óptica coincide con laMúltiplo entero de la longitud de onda, se produce resonancia, mientras que en la otra longitud de onda, la onda luminosa disminuye al redondear. Este documento presenta varios métodos experimentales para preparar microesferas para resonadores WGM a partir de polímeros conjugados en disolución: difusión de vapor 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 , mini-emulsión 31 y precipitación en interfase 32 . Cada método tiene características únicas; Por ejemplo, el método de difusión de vapor proporciona microesferas bien definidas con esfericidad muy alta y superficies lisas, pero sólo polímeros de baja cristalinidad pueden formar estas microesferas. Por otra parte, para la mini-emulsión, Varios tipos de polímeros conjugados, incluyendo polímeros de alta cristalina, pueden formar esferas, pero la morfología superficial es inferior a la obtenida a partir del método de difusión de vapor. El método de precipitación de interfases es preferible para crear microesferas a partir de polímeros no conjugados dopados con colorante. En todos los casos, la selección del disolvente y del no disolvente juega un papel importante en la formación de la morfología esférica. En la segunda mitad de este trabajo se presentan técnicas de micro-manipulación y μ-PL. Para la técnica μ-PL, se dispersan microesferas sobre un sustrato, y se utiliza un haz láser enfocado, a través de una lente de microscopio, para irradiar una única microesfera aislada 24 . El PL generado desde una esfera es detectado por un espectrómetro a través de la lente del microscopio. Mover la etapa de muestreo puede variar la posición del punto de excitación. El punto de detección también es variable inclinando la óptica del colimador de la excitaciónTación con respecto al eje óptico de la trayectoria de detección 28 , 32 . Para investigar la propagación de luz intersphere y la conversión de longitud de onda, la técnica de micro-manipulación se puede utilizar [ 32] . Para conectar varias microesferas con diferentes propiedades ópticas, es posible recoger una esfera utilizando una microaguja y colocarla en otra esfera. Conjuntamente con las técnicas de micromanipulación y el método μ-PL, se pueden realizar diversas mediciones ópticas utilizando esferas de polímero conjugado, que se preparan mediante un método de autoensamblaje simple. Este documento de vídeo será útil para los lectores que deseen utilizar materiales poliméricos blandos para aplicaciones ópticas.

<table border="1" fo:keep-together.within-page="1" fo:keep-with-next.within-page="always">
	<tbody>
		<tr>
			<td>polystyrene</td>
			<td>Aldrich</td>
			<td>132427-25G</td>
			<td></td>
		</tr>
		<tr>
			<td>sodium dodecylsulfate</td>
			<td>Kanto Kagaku</td>
			<td>372035-31</td>
			<td></td>
		</tr>
		<tr>
			<td>tetrahydrofuran</td>
			<td>Wako</td>
			<td>206-08744</td>
			<td></td>
		</tr>
		<tr>
			<td>chloroform</td>
			<td>Wako</td>
			<td>038-18495</td>
			<td></td>
		</tr>
		<tr>
			<td>methanol</td>
			<td>Wako</td>
			<td>139-13995</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly(9,9-di-n-octylfluorenyl-2,7-diyl)</td>
			<td>Aldrich</td>
			<td>571652-500MG</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly[2-methoxy-5-(3&#8242;,7&#8242;-dimethyloctyloxy)-1,4-phenylenevinylene] (MDMOPPV)</td>
			<td>Aldrich</td>
			<td>546461-1G</td>
			<td></td>
		</tr>
		<tr>
			<td>poly[(9,9-dioctylfluorene-2,7-diyl)-alt-(5-octylthieno[3,4-c]pyrrole-4,6-dione-1,3-diyl)] (P1)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 28</td>
		</tr>
		<tr>
			<td>poly[(N-(2-heptylundecyl)carbazole-2,7-diyl)-alt-(4,8-bis[(dodecyl)carbonyl]benzo[1,2-b:4,5-b&#8242;]dithiophene-2,6-diyl)] (P2)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 28</td>
		</tr>
		<tr>
			<td>fluorescent dye (boron dipyrrin; BODIPY)</td>
			<td>synthesized</td>
			<td>-</td>
			<td>reference 32</td>
		</tr>
		<tr>
			<td>Optical Microscope</td>
			<td>Nicon</td>
			<td>Eclipse LV-N</td>
			<td></td>
		</tr>
		<tr>
			<td>laser_405 nm</td>
			<td>Hutech</td>
			<td>DH405-10-5</td>
			<td></td>
		</tr>
		<tr>
			<td>laser_355 nm</td>
			<td>CNI</td>
			<td>MPL-F-355-10&#65357;W</td>
			<td></td>
		</tr>
		<tr>
			<td>Spectrometer</td>
			<td>Lambda Vision</td>
			<td>LV-MC3/T</td>
			<td></td>
		</tr>
		<tr>
			<td>Homogenizer</td>
			<td>Microtech Nichion</td>
			<td>Physcotron NS-360D</td>
			<td></td>
		</tr>
		<tr>
			<td>micromanipulation</td>
			<td>Microsupport</td>
			<td>Quick Pro QP-3RH</td>
			<td></td>
		</tr>
	</tbody>
</table>

fabrication of polymer microspheres for optical resonator and laser applications

Este documento describe tres métodos de preparación de microesferas fluorescentes que comprenden polímeros conjugados o no conjugados: difusión de vapor, precipitación en interfase y mini-emulsión. En todos los métodos, se obtienen esferas bien definidas de tamaño micrométrico a partir de un proceso de autoensamblaje en solución. El método de difusión de vapor puede dar lugar a esferas con la mayor esfericidad y suavidad superficial, aunque los tipos de polímeros capaces de formar estas esferas son limitados. Por otra parte, en el método de mini-emulsión, las microesferas se pueden fabricar a partir de diversos tipos de polímeros, incluso de polímeros altamente cristalinos con espinas dorsales coplanares, conjugadas con π. Las propiedades fotoluminiscentes (PL) de las microesferas aisladas aisladas son inusuales: la PL está confinada dentro de las esferas, se propaga en la circunferencia de las esferas a través de la reflexión interna total en la interfase polımero / aire y se autointerfiere para mostrar resonancias agudas y periódicas Líneas PL. Estos resonanciaG son los denominados &quot;modos de galería susurrantes&quot; (WGMs). Este trabajo demuestra cómo medir WGM PL a partir de esferas aisladas aisladas utilizando la técnica de micro-fotoluminiscencia (μ-PL). En esta técnica, un rayo láser enfocado irradia una sola microesfera, y la luminescencia es detectada por un espectrómetro. A continuación, se utiliza una técnica de micromanipulación para conectar las microesferas una a una y para demostrar la propagación de la intersphere PL y la conversión de color a partir de microesferas acopladas por excitación en el perímetro de una esfera y detección de PL desde la otra microesfera. Estas técnicas, μ-PL y micromanipulación, son útiles para experimentos en aplicaciones de micro-óptica utilizando materiales poliméricos.

La Figura 1 muestra representaciones esquemáticas del método de difusión de vapor (a), método de mini-emulsión (b) y método de precipitación de interfaz (c). Para el método de difusión de vapor ( Figura 1a ), se colocó un vial de 5 ml que contenía una solución de polímeros de CHCl $ ₃ $ (0,5 mg ml -1 , 2 ml) en un vial de 50 ml que contenía 5 ml de un no disolvente, tal como MeOH . El vial exterior se tapó y después se dejó reposar durante 3 días a 25ºC. El vapor del no disolvente se difunde lentamente en la solución, dando como resultado la precipitación de los polímeros a través del estado sobresaturado. Para el método de mini-emulsión ( Figura 1b ), se añadió una solución de CHCl3 de polímeros (5 mg ml -1 , 200 μl) a una solución acuosa de n- dodecilsulfato sódico (SDS, 1 mM, 2 ml). La disolución separada en dos fases de agua / CHCl $ ³ $ fue emulsiSe sometió a agitación vigorosa con un homogeneizador (30.000 rpm, 5 min). La emulsión resultante se dejó reposar durante 24 horas a 25ºC y 1 atm para evaporar naturalmente el CHCl $ ₃ $. El exceso de SDS se eliminó intercambiando el agua sobrenadante por centrifugación (3 veces) para obtener un precipitado de polímeros conjugados. Para el método de precipitación de interfase ( Figura 1c ), una solución de THF de una mezcla de poliestireno (PS, [PS] = 1,0 mg ml -1 ) y colorante fluorescente ([colorante] = 0,002-1,0 mg mL -1 = 6,4-3,200 ΜM) a la capa no disolvente de una mezcla agua / EtOH (6/1 v / v, 1 ml). La difusión lenta de los disolventes, junto con la evaporación simultánea de THF al aire, resultó en precipitación después de 6 h de envejecimiento. Las micrografías de microscopía electrónica de barrido (SEM) de las microesferas resultantes preparadas por cada método se muestran en la figuraUre 1. Para los métodos de difusión de vapor y precipitación de interfases, se obtuvieron microesferas bien definidas con esfericidad alta y superficies lisas. Por otra parte, para el método de mini-emulsión, se obtuvieron microesferas bien definidas, pero la morfología superficial no fue tan suave en comparación con las producidas por los otros métodos. Esto se debe a que el tensioactivo cubre toda la superficie de las microesferas. Sin embargo, el mérito del método de mini-emulsión es que las microesferas se pueden fabricar a partir de diversos tipos de polímeros conjugados. Esto es bastante ventajoso porque, con el método de difusión de vapor, los polímeros con alta cristalinidad apenas forman geometría esférica. En el método de precipitación de interfase, el agua se usa a menudo como un no disolvente en la capa inferior. Sin embargo, los polímeros conjugados con π son usualmente muy hidrófobos, de manera que se produce una aglomeración pesada de las microesferas resultantes. Esto es desventajoso para aislar cada microesfera sobre un sustrato para μ-PL meAsurements. La figura 2 muestra una representación esquemática de la configuración experimental μ-PL. Se utilizó un microscopio óptico con un objetivo de 50X o 100X para identificar partículas adecuadas y determinar sus diámetros ( d ). Para las mediciones, se utilizó un sistema μ-PL con un microscopio combinado con un monocromador (rejilla: 300 ó 1.200 ranuras mm -1 ) y una cámara CCD. El perımetro de una sola microesfera se fotoexcitó a 25 ◦ C bajo condiciones ambientales mediante un láser cw o pulsado con una longitud de onda de excitación (λex) de 405 nm (cw), 532 nm (cw), 355 nm (láser de pulso, frecuencia, 1 kHz, duración del impulso, 7 ns), o 470 nm (láser de pulso, frecuencia, 2,5 MHz, duración del impulso, 70 ps). Para las mediciones de μ-PL con diferentes posiciones de excitación y detección, las esferas fueron excitadas por un láser de 405 nm,Y la luz se recogió en una configuración confocal por un objetivo 50X y detectado por un espectrómetro con una rejilla de 300 ranuras mm -1 . El tamaño del punto, la potencia del láser y el tiempo de integración fueron de 0,5 μm, 0,5 μW y 1 s, respectivamente. Para separar el punto de detección de la excitación, la óptica colimadora del haz de láser de excitación se inclinó con respecto al eje óptico de la trayectoria de detección. La Figura 3 muestra el WGM PL de una única microesfera de polímeros conjugados con π: P1 16k , P2 , y sus mezclas. Se observaron espectros de WGM PL transparentes de todas las microesferas individuales. El factor Q, definido por una longitud de onda pico dividida por la mitad del ancho del pico, alcanzó hasta 2,200 para microesferas de P1 16k , mientras que las microesferas de P2 mostraron un factor Q de sólo 300, posibleY debido a la morfología superficial rugosa [ 28] . Para las microesferas de mezcla de polímeros, se produjo transferencia de energía intrasférica eficiente, dando lugar a un cambio significativo del WGM PL de una región de color amarillo a una de color rojo. Se mantuvo un alto factor Q (1.500) debido a la superficie lisa. Además, la cascada de transferencia de energía intersférica se investigó mediante una combinación de técnicas de micro-manipulación y μ-PL. Así, las microesferas PS polimórficas de boro-dipirina (BODIPY) con colores PL de verde, amarillo, naranja y rojo se conectaron una a una para formar tetrasferias con configuraciones lineales y en forma de T ( Figura 4 ) 32 . El análisis detallado de la eficiencia de transferencia de energía indicó que la transferencia de energía de luz de verde a amarillo y de amarillo a naranja se llevó a cabo de manera eficiente, mientras que la transferencia de energía de naranja a rojo apenas ocurría b<html> Debido a la pequeña superposición entre la banda PL del donante de energía y la banda de absorción del aceptor de energía. Huelga decir que las transferencias de energía convertidas, como las de rojo a naranja, amarillo y verde, apenas se produjeron. <img alt="Figura 1" class="xfigimg" src="/files/ftp_upload/55934/55934fig1.jpg" /> Figura 1: Método de preparación de microesferas de polímero. Representaciones esquemáticas del método de difusión de vapor ( a ), método de mini-emulsión ( b ), y método de precipitación de interfase ( c ) y micrografías SEM de las microesferas de polímero resultantes de cada método de preparación. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig1large.jpg" target="_blank">Haga clic aquí para ver una versión más grande de esta figura.</a> 55934fig2.jpg &quot;/&gt; Figura 2: Representación esquemática de la configuración experimental para mediciones μ-PL. <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig2large.jpg" target="_blank">Haga clic aquí para ver una versión más grande de esta figura.</a> <img alt="figura 3" class="xfigimg" src="/files/ftp_upload/55934/55934fig3.jpg" /> Figura 3: Espectros PL de una sola microesfera. (A) Estructuras moleculares de P1 16k y P2 y representaciones esquemáticas de las microesferas autoensambladas de P1 16k , P2 , y su mezcla ( P1 16k / P2 = 8/2 p / p), junto con sus micrografías SEM. ( B - d ) espectros PL de una sola microesfera formada a partir de P1 16k ( b ),<html> P1 16k / P2 mezcla ( c ), y P2 ( d ). <a href="https://ecsource-jove-com.remotexs.ntu.edu.sg/files/ftp_upload/55934/55934fig3large.jpg" target="_blank">Haga clic aquí para ver una versión más grande de esta figura.</a> <img alt="Figura 4" class="xfigimg" src="/files/ftp_upload/55934/55934fig4.jpg" /> Figura 4: Técnica de micromanipulación para disponer las microesferas. (A) Micrografía óptica de microesferas PS polimórficas dopadas con BODIPY, manipuladas por una micro-aguja delgada. ( B) y c ) Micrografías ópticas (arriba) y fluorescentes (abajo) de las microesferas conectadas con configuraciones lineales ( b ) y en forma de T ( c ). ( D ) Representación esquemática de la transferencia de energía intersférica mediada por cavidades.Jpg &quot;target =&quot; _ blank &quot;&gt; Haga clic aquí para ver una versión más grande de esta figura.

Watch this Scientific Journal Video about Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications at JoVE.com

Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

Se presentan protocolos para la síntesis de microesferas a partir de polímeros, la manipulación de microesferas y medidas de micro-fotoluminiscencia.

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, ...

fabrication-polymer-microspheres-for-optical-resonator-laser

Nanyang Technological University

Research

JoVE Journal

Engineering

13.9K vistas.  University of Tsukuba.  Se presentan protocolos para la síntesis de microesferas a partir de polímeros, la manipulación de microesferas y medidas de micro-fotoluminiscencia. 

Video: Fabrication of Polymer Microspheres for Optical Resonator and Laser Applications

Construction and Testing of Coin Cells of Lithium Ion Batteries

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime. Lithium ion batteries have also been considered to be used in electric and hybrid vehicles1 or even electrical grid stabilization systems2. All these applications simulate a dramatic increase in the research and development of battery materials3-7, including new materials3,8, doping9, nanostructuring10-13, coatings or surface modifications14-17 and novel binders18. Consequently, an increasing number of physicists, chemists and materials scientists have recently ventured into this area. Coin cells are widely used in research laboratories to test new battery materials; even for the research and development that target large-scale and high-power applications, small coin cells are often used to test the capacities and rate capabilities of new materials in the initial stage. 
 In 2010, we started a National Science Foundation (NSF) sponsored research project to investigate the surface adsorption and disordering in battery materials (grant no. DMR-1006515). In the initial stage of this project, we have struggled to learn the techniques of assembling and testing coin cells, which cannot be achieved without numerous help of other researchers in other universities (through frequent calls, email exchanges and two site visits). Thus, we feel that it is beneficial to document, by both text and video, a protocol of assembling and testing a coin cell, which will help other new researchers in this field. This effort represents the "Broader Impact" activities of our NSF project, and it will also help to educate and inspire students.
In this video article, we document a protocol to assemble a CR2032 coin cell with a LiCoO2 working electrode, a Li counter electrode, and (the mostly commonly used) polyvinylidene fluoride (PVDF) binder. To ensure new learners to readily repeat the protocol, we keep the protocol as specific and explicit as we can. However, it is important to note that in specific research and development work, many parameters adopted here can be varied. First, one can make coin cells of different sizes and test the working electrode against a counter electrode other than Li. Second, the amounts of C black and binder added into the working electrodes are often varied to suit the particular purpose of research; for example, large amounts of C black or even inert powder were added to the working electrode to test the "intrinsic" performance of cathode materials14. Third, better binders (other than PVDF) have also developed and used18. Finally, other types of electrolytes (instead of LiPF6) can also be used; in fact, certain high-voltage electrode materials will require the uses of special electrolytes7.

A protocol to construct and test coin cells of lithium ion batteries is described. The specific procedures of making a working electrode, preparing a counter electrode, assembling a cell inside a glovebox and testing the cell are presented.

Construcción y verificación de las células de la moneda de baterías de ion de litio

Rechargeable lithium ion batteries have wide applications in electronics, where customers always demand more capacity and longer lifetime.  Lithium ion ...

Investigación

Ingeniería

Fabrication of Nano-engineered Transparent Conducting Oxides by Pulsed Laser Deposition

Nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas allows the deposition of metal oxides with tunable morphology, structure, density and stoichiometry by a proper control of the plasma plume expansion dynamics. Such versatility can be exploited to produce nanostructured films from compact and dense to nanoporous characterized by a hierarchical assembly of nano-sized clusters. In particular we describe the detailed methodology to fabricate two types of Al-doped ZnO (AZO) films as transparent electrodes in photovoltaic devices: 1) at low O2 pressure, compact films with electrical conductivity and optical transparency close to the state of the art transparent conducting oxides (TCO) can be deposited at room temperature, to be compatible with thermally sensitive materials such as polymers used in organic photovoltaics (OPVs); 2) highly light scattering hierarchical structures resembling a forest of nano-trees are produced at higher pressures. Such structures show high Haze factor (&gt;80%) and may be exploited to enhance the light trapping capability. The method here described for AZO films can be applied to other metal oxides relevant for technological applications such as TiO2, Al2O3, WO3 and Ag4O4.

We describe the experimental method to deposit nanostructured oxide thin films by nanosecond Pulsed Laser Deposition (PLD) in the presence of a background gas. By using this method Al-doped ZnO (AZO) films, from compact to hierarchically structured as nano-tree forests, can be deposited.

La fabricación de nano-ingeniería óxidos conductores transparentes por deposición por láser pulsado

Nanosecond Pulsed  Laser Deposition (PLD) in the presence of a background gas allows the deposition  of metal oxides with tunable morphology, structure, ...

Fabrication and Characterization of Disordered Polymer Optical Fibers for Transverse Anderson Localization of Light

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed polymer optical fiber is composed of 80,000 strands of poly (methyl methacrylate) (PMMA) and polystyrene (PS) that are randomly mixed and drawn into a square cross section optical fiber with a side width of 250 &mu;m. Initially, each strand is 200 &mu;m in diameter and 8-inches long. During the mixing process of the original fiber strands, the fibers cross over each other; however, a large draw ratio guarantees that the refractive index profile is invariant along the length of the fiber for several tens of centimeters. The large refractive index difference of 0.1 between the disordered sites results in a small localized beam radius that is comparable to the beam radius of conventional optical fibers. The input light is launched from a standard single mode optical fiber using the butt-coupling method and the near-field output beam from the disordered fiber is imaged using a 40X objective and a CCD camera. The output beam diameter agrees well with the expected results from the numerical simulations. The disordered optical fiber presented in this work is the first device-level implementation of 2D Anderson localization, and can potentially be used for image transport and short-haul optical communication systems.

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. This microstructured fiber can transport a small localized beam with a radius that is comparable to the beam radius of conventional optical fibers.

Fabricación y Caracterización de Polímeros desordenados Fibras ópticas para Transversal Anderson Localización de Luz

We develop and characterize a disordered polymer optical fiber that uses transverse Anderson localization as a novel waveguiding mechanism. The developed ...

Patterning via Optical Saturable Transitions - Fabrication and Characterization

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical Saturable Transitions (POST). In this technique the chemical properties of organic photochromic molecules that undergo single-photon reactions are exploited, enabling rapid top-down nanopatterning over large areas at low light intensities, thereby, allowing for the circumvention of the far-field diffraction barrier.4 Simple, cost-effective, high throughput and resolution alternatives to nanopatterning are being explored, such as, two-photon polymerization5,6, beam pen lithography (BPL)7, scanning electron beam lithography (SEBL), and focused ion beam (FIB) patterning. However, multi-photon approaches require high light intensities, which limit their potential for high throughput and offer low image contrast. Although, electron and ion beam lithographic processes offer increased resolution, the serial nature of the process is limited to slow writing speeds, which also prevents patterning of features over large areas. Beam-pen lithography is an approach towards parallel near-field optical lithography. However, the gap between the source of the beam and the surface of the photoresist needs to be controlled extremely precisely for good pattern uniformity and this is very challenging to accomplish for large arrays of beams. Patterning via Optical Saturable Transitions (POST) is an alternative optical nanopatterning technique for patterning sub-wavelength features1-3. Since this technique uses single photons instead of electrons, it is extremely fast and does not require high light intensities1-3, opening the door to massive parallelization.

We report that the diffraction limit of conventional optical lithography can be overcome by exploiting the transitions of organic photochromic derivatives induced by their photoisomerization at low light intensities.1-3 This paper outlines our fabrication technique and two locking mechanisms, namely: dissolution of one photoisomer and electrochemical oxidation.

Patrones través ópticos saturable Transiciones - Fabricación y Caracterización

This protocol describes the fabrication and characterization of nanostructures using a novel nanolithographic technique called Patterning via Optical ...

Fabrication and Operation of a Nano-Optical Conveyor Belt

The technique of using focused laser beams to trap and exert forces on small particles has enabled many pivotal discoveries in the nanoscale biological and physical sciences over the past few decades. The progress made in this field invites further study of even smaller systems and at a larger scale, with tools that could be distributed more easily and made more widely available. Unfortunately, the fundamental laws of diffraction limit the minimum size of the focal spot of a laser beam, which makes particles smaller than a half-wavelength in diameter hard to trap and generally prevents an operator from discriminating between particles which are closer together than one half-wavelength. This precludes the optical manipulation of many closely-spaced nanoparticles and&#160;limits the&#160;resolution of optical-mechanical systems. Furthermore, manipulation using focused beams requires beam-forming or steering optics, which can be very bulky and expensive. To address these limitations in the system scalability of conventional optical trapping our lab has devised an alternative technique which utilizes near-field optics to move particles across a chip. Instead of focusing laser beams in the far-field, the optical near field of plasmonic resonators produces the necessary local optical intensity enhancement to overcome the restrictions of diffraction and manipulate particles at higher resolution. Closely-spaced resonators produce strong optical traps which can be addressed to mediate the hand-off of particles from one to the next in a conveyor-belt-like fashion. Here, we describe how to design and produce a conveyor belt using a gold surface patterned with plasmonic C-shaped resonators and how to operate it with polarized laser light to achieve super-resolution nanoparticle manipulation and transport. The nano-optical conveyor belt chip can be produced using lithography techniques and easily packaged and distributed.

The scalability and resolution of conventional optical manipulation techniques are limited by diffraction. We circumvent the diffraction limit and describe a method of optically transporting nanoparticles across a chip using a gold surface patterned with a path of closely spaced C-shaped plasmonic resonators.

Fabricación y operación de una banda transportadora nano-óptica

The technique of using focused laser beams to trap and exert forces on small particles has enabled many pivotal discoveries in the nanoscale biological ...

Compact Lens-less Digital Holographic Microscope for MEMS Inspection and Characterization

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and automotive. However, effective inspection and characterization metrology systems are needed to ensure the functional reliability of MEMS. This study presents a system based on digital holography as a tool for MEMS metrology. Digital holography has gained increasing attention in the past 20 years. With the fast development and decreasing cost of sensor arrays, resolution of such systems has increased broadening potential applications. Thus, it has attracted attention from both research and industry sides as a potential reliable tool for industrial metrology. Indeed, by recording the interference pattern between an object beam (which contains sample height information) and a reference beam on a CCD camera, one can retrieve the quantitative phase information of an object. However, most of digital holographic systems are bulky and thus not easy to implement on industry production lines. The novelty of the system presented is that it is lens-less and thus very compact. In this study, it is shown that the Compact Digital Holographic Microscope (CDHM) can be used to evaluate several characteristics typically consider as criteria in MEMS inspections. The surface profiles of MEMS in both static and dynamic conditions are presented. Comparison with AFM is investigated to validate the accuracy of the CDHM.

We present a compact reflection digital holographic system (CDHM) for inspection and characterization of MEMS devices. A lens-less design using a diverging input wave providing natural geometrical magnification is demonstrated. Both static and dynamic studies are presented.

Compacto holográfica microscopio digital Lente menos por MEMS Inspección y Caracterización

A micro-electro-mechanical-system (MEMS) is a widely used component in many industries, including energy, biotechnology, medical, communications, and ...

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 ...

Fabrication of 1-D Photonic Crystal Cavity on a Nanofiber Using Femtosecond Laser-induced Ablation

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using femtosecond laser-induced ablation. We show that thousands of periodic nano-craters are fabricated on an optical nanofiber by irradiating with just a single femtosecond laser pulse. For a typical sample, periodic nano-craters with a period of 350 nm and with diameter gradually varying from 50 - 250 nm over a length of 1 mm are fabricated on a nanofiber with diameter around 450 - 550 nm. A key aspect of such a nanofabrication is that the nanofiber itself acts as a cylindrical lens and focuses the femtosecond laser beam on its shadow surface. Moreover, the single-shot fabrication makes it immune to mechanical instabilities and other fabrication imperfections. Such periodic nano-craters on nanofiber, act as a 1-D PhC and enable strong and broadband reflection while maintaining the high transmission out of the stopband. We also present a method to control the profile of the nano-crater array to fabricate apodized and defect-induced PhC cavities on the nanofiber. The strong confinement of the field, both transverse and longitudinal, in the nanofiber-based PhC cavities and the efficient integration to the fiber networks, may open new possibilities for nanophotonic applications and quantum information science.

We present a protocol for fabricating 1-D photonic crystal cavities on subwavelength diameter silica fibers (optical nanofibers) using femtosecond laser-induced ablation.

La fabricación de 1-D de cristal fotónico cavidad en un nanofibras Uso de ablación inducida por láser de femtosegundo

We present a protocol for fabricating 1-D Photonic Crystal (PhC) cavities on subwavelength-diameter tapered optical fibers, optical nanofibers, using ...

Fabrication of Superhydrophobic Metal Surfaces for Anti-Icing Applications

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in industry. The wettability of the produced surface was analyzed by bouncing drop experiments and the topography was analyzed by confocal microscopy. In addition, we show various methodologies to measure its durability and anti-icing properties. Superhydrophobic surfaces hold a special texture that must be preserved to keep their water-repellency. To fabricate durable surfaces, we followed two strategies to incorporate a resistant texture. The first strategy is a direct incorporation of roughness to the metal substrate by acid etching. After this surface texturization, the surface energy was decreased by silanization or fluoropolymer deposition. The second strategy is the growth of a ceria layer (after surface texturization) that should enhance the surface hardness and corrosion resistance. The surface energy was decreased with a stearic acid film.
The durability of the superhydrophobic surfaces was examined by a particle impact test, mechanical wear by lateral abrasion, and UV-ozone resistance. The anti-icing properties were explored by studying the ability to repeal subcooled water, freezing delay, and ice adhesion.

We illustrate several methodologies to produce superhydrophobic metal surfaces and to explore their durability and anti-icing properties.

Fabricación de superficies metálicas superhidrófobos para aplicaciones anti-hielo

Several ways to produce superhydrophobic metal surfaces are presented in this work. Aluminum was chosen as the metal substrate due to its wide use in ...

Fused Filament Fabrication (FFF) of Metal-Ceramic Components

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with diverse customization options and favorable production methods is increasing continuously. With fused filament fabrication (FFF), it is possible to produce large and complex components quickly with high material efficiency. In FFF, a continuous thermoplastic filament is melted in a heated nozzle and deposited below. The computer-controlled print head is moved in order to build up the desired shape layer by layer. Investigations regarding printing of metals or ceramics are increasing more and more in research and industry. This study focuses on additive manufacturing (AM) with a multi-material approach to combine a metal (stainless steel) with a technical ceramic (zirconia: ZrO2). Combining these materials offers a broad variety of applications due to their different electrical and mechanical properties. The paper shows the main issues in preparation of the material and feedstock, device development, and printing of these composites.

Fused Filament Fabrication FFF of Metal-Ceramic Components

This study shows multi-material additive manufacturing (AM) using fused filament fabrication (FFF) of stainless steel and zirconia.

Fabricación de filamento fundido (FFF) de componentes de Metal-cerámica

Technical ceramics are widely used for industrial and research applications, as well as for consumer goods. Today, the demand for complex geometries with ...