Name: layer-by-layer synthesis and transfer of freestanding conjugated microporous polymer nanomembranes
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1. Síntesis de CMP Thin Films través de la adición secuencial <ol><li> Autoensamblada monocapa (SAM) funcionalización de oro sobre mica. <ol><li> Prepare la solución 1 mM de 11-tioacetilo-undecano amida de ácido propargılico 14 en etanol (SAM-solución). Mezclar mediante baño ultrasónico hasta que la solución es clara. Proteja la botella de la luz usando papel de aluminio. </li><li> Obtener oro mica recubierta de obleas en atmósfera de argón. Después de la retirada del recipiente de alma...

<ol>
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A., W&#246;ll, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=MOF+thin+films:+existing+and+future+applications.">MOF thin films: existing and future applications.</a> Chemical Society Reviews. 40 (2), 1081-1106 (2011).</li><li>Liu, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Deposition+of+Metal-Organic+Frameworks+by+Liquid-Phase+Epitaxy:+The+Influence+of+Substrate+Functional+Group+Density+on+Film+Orientation.">Deposition of Metal-Organic Frameworks by Liquid-Phase Epitaxy: The Influence of Substrate Functional Group Density on Film Orientation.</a> Materials. 5 (9), 1581-1592 (2012).</li><li>Such, G. K., Quinn, J. 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Para la síntesis de la CMP-película de la solución del catalizador tiene que ser fresco. Un catalizador roto (es decir, oxidada) se indica mediante una coloración azul de la solución. La solución fresca es incoloro. Un punto crucial es cortar los bordes del sustrato mica después de revestimiento por rotación PMMA. También defectos en el sustrato se deben cortar, es decir, cada punto fuera el PMMA pueda entrar en contacto con el sustrato de mica, a causa de...

The preparation of ultra-thin polymer membranes is of high interest for applications in gas separation and nanofiltration. Challenges in the synthesis are represented by (a) the control of the membrane thickness and the homogeneity and (b) transfer of such fragile membranes. To overcome challenge (a), molecular layer-by-layer synthesis1 has shown great promise in controlling the thickness and homogeneity of thin films grown at the solid-liquid interface.2,3 Controlling the number of layers linearly controls the film thickness. The l-b-l method has been successfully used to fabricate surface mounted metal organic frameworks (SURMOFs),4-7 also the synthesis of thin polymer films via l-b-l reaction of polymer chains was demonstrated.8 The challenge (b) concerns the handling of these ultra-thin membranes. To avoid rupture or wrinkling of the nanomembranes sacrificial supports of coatings have shown great promise. 9
Here we will present a detailed protocol for synthesis of conjugated microporous polymer (CMP)10-13 thin films through sequential addition of the molecular building blocks, with desired thickness and composition. The preparation of free-standing CMP nanomembranes is achieved by using a sacrificial support. To handle and transfer the CMP nanomembranes to other supports we will describe a simple protocol to protect the membranes with sacrificial coatings and their upfloating to the liquid air interface and subsequent transfer using dip-coating.

<table>
	<tbody>
		<tr>
			<td>Acetone</td>
			<td>VWR BDH Prolabo</td>
			<td>20066.330</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Potassium iodide</td>
			<td>VWR BDH Prolabo</td>
			<td>26846.292</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Ethyl acetate</td>
			<td>VWR BDH Prolabo</td>
			<td>23882.321</td>
			<td>AnalR NORMAPUR</td>
		</tr>
		<tr>
			<td>Tetrahydrofurane (THF)</td>
			<td>VWR BDH Prolabo</td>
			<td>28559.320</td>
			<td>HiPerSolv CHROMANORM</td>
		</tr>
		<tr>
			<td>THF waterfree</td>
			<td>Merck Millipore</td>
			<td>1.08107.1001</td>
			<td>SeccoSolv</td>
		</tr>
		<tr>
			<td>Iodine</td>
			<td>Sigma-Aldrich</td>
			<td>20,777-2</td>
			<td></td>
		</tr>
		<tr>
			<td>Tetrakis(acetonitrile)copper(I)hexafluoro-phosphate</td>
			<td>Sigma-Aldrich</td>
			<td>346276-5G</td>
			<td></td>
		</tr>
		<tr>
			<td>Poly(methyl methacrylate) 996 kDa (PMMA)</td>
			<td>Sigma-Aldrich</td>
			<td>182265-25G</td>
			<td></td>
		</tr>
		<tr>
			<td>1.1.1.1 Methanetetrayltetrakis(4-azidobenzene) (TPM-azide)</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to9</td>
		</tr>
		<tr>
			<td>1.1.1.1 Methanetetrayltetrakis(4-ethinylenebenzene) (TPM-alkyne)</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to9</td>
		</tr>
		<tr>
			<td>11-thioacetyl-undecaneacid propargylamide</td>
			<td></td>
			<td></td>
			<td>provided by AK Prof. Br&#228;se. Institute of organic chemistry, Karlsruhe Institute of Technology. Synthesized according to8</td>
		</tr>
		<tr>
			<td>gold/titan coated silicium-wafer</td>
			<td>Georg Albert PVD, 76857 Silz, Germany</td>
			<td></td>
			<td></td>
		</tr>
		<tr>
			<td>gold coated mica</td>
			<td>Georg Albert PVD, 76857 Silz, Germany</td>
			<td></td>
			<td></td>
		</tr>
	</tbody>
</table>

layer-by-layer synthesis and transfer of freestanding conjugated microporous polymer nanomembranes

CMP como grandes materiales de área superficial han atraído creciente interés recientemente, debido a su alta variabilidad en la incorporación de grupos funcionales en combinación con su sobresaliente estabilidad térmica y química, y densidades bajas. Sin embargo, su naturaleza insoluble causa problemas en su procesamiento ya que las técnicas generalmente aplicados como recubrimiento por centrifugación no están disponibles. Especialmente para aplicaciones de membrana, en las que es deseable la tramitación de CMP como películas delgadas, los problemas de procesamiento han impedido su aplicación comercial. Aquí se describe la síntesis interfacial de CMP películas delgadas sobre sustratos funcionalizados vía (LBL) la síntesis molecular capa por capa. Este proceso permite la preparación de películas con grosor y la composición deseada y los gradientes de composición incluso deseados. El uso de soportes de sacrificio permite la preparación de membranas Autosoportados por disolución del soporte después dela síntesis. Para manejar este tipo de membranas independientes ultrafinas la protección con recubrimientos de sacrificio mostró una gran promesa, para evitar la rotura de las nanomembranes. Para transferir los nanomembranes al sustrato deseado, las membranas revestidas se upfloated en la interfase aire-líquido y luego se transfieren a través de recubrimiento por inmersión.

Las membranas se caracterizan por espectroscopia de absorción reflexión de infrarrojos (IRRAS). 16 La Figura 4 muestra IRRA-espectros a partir de una CMP-membrana transferido a una oblea de oro. Bandas típicas de las vibraciones de la columna vertebral aromático están a 1.605 cm -1, 1.515 cm -1 y 1.412 cm -1. Grupos alquino y azida sin reaccionar pueden ser observados por bandas características a 2.125 cm -1 y 1.227 cm-1. La...

Watch this Scientific Journal Video about Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes at JoVE.com

Layer-by-layer Synthesis and Transfer of Freestanding Conjugated Microporous Polymer Nanomembranes

In this paper we describe the interfacial synthesis of conjugated microporous polymers (CMP) on sacrificial substrates, and the dissolution of the substrate for the preparation of freestanding CMP nanomembranes. In addition, we will describe how the fragile nanomembranes can be transferred to other substrates.

Síntesis de capa por capa y Transferencia de Independientes conjugados microporosas de polímero nanomembranes

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