Name: fabrication of large-area free-standing ultrathin polymer films
Uploaded: 2015-06-03T14:00:00.000+00:00
Duration: 10 min 8 s
Description: Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

Este trabalho realizado sob os auspícios do Departamento de Energia dos EUA por Lawrence Livermore National Laboratory sob contrato DE-AC52-07NA27344.

1. Preparação de Soluções <ol><li> Filtre a 60 g de lactato de etilo, utilizando uma seringa e um filtro de seringa 0,20 uM. Adicionar 0,3 g de polivinil formal ao lactato de etilo. Colocar a solução no forno a 50 ° C durante 4 h. Agitar suavemente o frasco para ver se o polímero se tenha dissolvido completamente. <ol><li> Se a solução estiver turva ou ainda mostra falta de homogeneidade ópticos, devolva o frasco ao forno por mais 2 horas. Esta receita é para uma solução de polímero de 0,5% em peso, que é tipicamente usado para espessuras de película de cerca de 30 nm. Soluções com maior teor de polímero pode ser usado para películas mais espessas. </li></ol></li><li> Prepara-se uma solução PDAC pesando 1,0 g de reagente de PDAC num balão volumétrico de 20 ml e enchendo o balão à linha de medição com água desionizada (Dl). Agite a solução suavemente antes de transferi-lo para um recipiente de armazenamento. </li></ol> 2. Preparação do Substrato <ol><li> CUIDADO. Colocar 60 ml de ácido sulfúrico concentradoácido em um copo de 250 ml limpo. Adiciona-se lentamente 20 ml de 30% de peróxido de hidrogénio. Espere até fumegante subsídios, em seguida, agite a solução suavemente. A solução e o copo irá tornar-se muito quente e a mistura é corrosiva. </li><li> Coloque um 150 milímetros placa de Petri sobre a placa quente e despeje o ácido no prato. Situado na placa quente a 100 ° C. <ol><li> Coloque uma pastilha de 4 &#39;de silício no ácido com o lado polido para cima. Empurre a bolacha para baixo no meio com um par de pinças para se certificar de toda a superfície é molhada. Deixar a bolacha no ácido durante 30 min. </li></ol></li><li> Remover a bolacha a partir do ácido com um par de pinças e enxaguar a frente e para trás da pastilha cuidadosamente com água desionizada a partir de uma garrafa de esguicho. A água deve folha fora em um padrão regular. Secar a bolacha em uma bancada limpa. </li><li> Lavar uma seringa descartável de 3 ml e um filtro de 0,2 um em primeiro lugar com água desionizada e depois com uma solução PDAC por puxar o líquido para dentro da seringa, a montagem do filtro, e on empurrar o líquido para fora através do filtro. </li><li> Montar um wafer limpo no revestidor de rotação. Elaborar 1,0-1,2 ml de solução PDAC para dentro da seringa e dispensar através do filtro para o meio da bolacha. Giram a 4.000 rpm por 15 segundos, em seguida, transferir o wafer de uma placa quente (pré-aquecido a 50 ° C) e deixe descansar por 30 s. </li><li> Lavar a camada de PDAC seca com água DI e deixe a bolacha seca na bancada limpa. </li></ol> Fabrication 3. Filme <ol><li> Coloque um wafer tratados com PDAC seco para o revestidor de rotação. </li><li> Lavar uma seringa descartável 3 ml e um filtro de 0,45 um com a solução de lactato de etilo utilizando o procedimento descrito em 2.4). </li><li> Depósito de 2,5 ml da solução de lactato de etilo através do filtro com a seringa no meio da bolacha e centrifugação durante 10 segundos a 200 rpm, em seguida, durante 3 segundos a 1700 rpm (dependendo da espessura da película desejada). Não deve haver um filme líquido uniforme sobre a bolacha. </li><li> Deixe secar filme da rotação coateraté estar visivelmente seco (tipicamente 10-15 min), em seguida, colocá-la numa placa de aquecimento (pré-aquecido a 50 ° C) durante 10 min. </li><li> Cortar os filmes em quadrados pequenos para o lançamento, geralmente de 2 cm x 2 cm, mas pode ser maior, dependendo do tamanho do suporte de filme utilizado (3.5.1-3.5.2). Como alternativa, fazer dois escribas para delaminating um filme de tamanho wafer-(3.5.3). Nota: suportes de filme padrão são 19 x 19 mm, com uma abertura circular de 13 mm de diâmetro no meio. Para filmes de tamanho wafer-, utilizar um aro de fio (por exemplo, fios de aço inoxidável formado num círculo) com um diâmetro que é um &quot;menor do que a bolacha. A abertura circular é escolhido porque os filmes normalmente absorver água durante a decolagem e swell. À medida que as películas secar sobre o suporte, a água é removida e o filme irá encolher. Uma abertura circular permite uma distribuição uniforme da tensão. <ol><li> Coloque a bolacha em um modelo de corte. Use um modelo quadrado sobre o qual todas as bordas são mais altos do que a bolacha para evitar que a linha reta edge usado para guiar a lâmina durante a traçagem de tocar na bolacha. Marcar as bordas em intervalos de 2 cm a guiar o posicionamento da vara durante o corte em cubos. Empurre o wafer contra duas bordas para alinhá-lo. </li><li> Coloque uma borda em linha reta ao longo de duas marcas de alinhamento, e desenhar uma lâmina de barbear suavemente ao longo da borda em linha reta para escriturário do filme. Aplique uma pressão suficiente para marcar o filme, mas não muito para marcar a própria bolacha e produzir partículas. Em filmes mais espessos, a linha de corte será claramente visível. </li><li> Para a decolagem de um filme em um pedaço de bolacha, escriba da borda wafer com uma lâmina de barbear. Entre os dois apartamentos no wafer, escrevente uma tira larga o suficiente para prender a bolacha na cremalheira e pinhão. </li></ol></li><li> Encha um prato de cultura de 190 mm x 100 com água DI. Prenda o wafer com o grande plano de um rack e pinhão montado em uma fase de inclinação e, lentamente, coloque-o na água DI. A película deve separar a partir da bolacha na linha de água. <ol><li> Continue baixando a WAFer a uma taxa que dá o tempo suficiente para separar película da bolacha, em vez de empurrar o interface de lift-off abaixo da linha de água. Quando a primeira linha de quadrados tem destacado da bolacha e está a flutuar na superfície, diminuindo a pausa da bolacha. Para um filme de tamanho wafer-, continuar a imersão do wafer até que o filme destaca completamente. </li><li> Mergulhe a cabeça do suporte de película na água e movê-lo por baixo do filme. Alinhe a borda do aro punho com uma das bordas de filmes e tocar o aro com o filme. Se for bem sucedido, o filme vai ficar com o aro. <ol><li> Para um filme wafer-size, coloque o aro de arame debaixo da secção descrito, apenas um centímetro de distância da borda. Certifique-se de que o aro está centrada debaixo do filme antes de iniciar a captura, mantendo uma certa distância entre borda do filme e borda aro para que o filme pode envolver em torno do aro e dobre sobre si mesmo. </li></ol></li><li> Retrair o aro lentamente da água a umaângulo de 35 °. Levante o filme fora da água muito lentamente. Nota: Para os filmes a menos do que 20 nm de espessura, depois de aumentar o ângulo de cerca de metade do filme foi retirado da água a cerca de 90 ° (isto é, perpendicular à superfície da água) para evitar puxar a película através do suporte. Ao mudar o ângulo de elevação para fora, faça-o lentamente para evitar puxar o filme através do aro. </li><li> Quando o aro se encontra totalmente retraído, colocá-lo para o lado para secar. Certifique-se a parte inferior do aro é livre de gotas antes de colocar o aro para baixo, e utilizar uma superfície curva (tal como uma bandeja bolacha) para evitar a criação de uma vedação de líquido entre a superfície e aro. </li><li> Se quadrados mais scribed permanecem na bolacha, continuar a descer a bolacha na água e repetir as etapas acima para 3.6.1-3.6.4 quadrados restantes. </li><li> Deixe-os filmes O seco / N. </li></ol></li></ol>

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Os autores não têm nada a revelar.

O tratamento do substrato PDAC é baseado em interacções electrostáticas auto-limitante, ou seja, os substratos de qualquer tamanho pode ser facilmente tratada, desde que eles são carregados negativamente (por exemplo, silício ou vidro). As Figuras 1-2 mostra muito grandes filmes finos (até 13 centímetros de diâmetro) fabricado usando este protocolo, com a única mudança sendo o volume de reagentes utilizados. O tamanho viável final parece ser limitada apenas pela deposição e delami...

Autónoma finas películas de polímero são utilizadas numa variedade de aplicações, incluindo sensores, 1-3 MEMs, catálise ou filtração, 4 e engenharia de tecidos. 5-8 Eles também são utilizados para estudos fundamentais que exploram o comportamento dos polímeros sob confinamento. 9- 13 Uma película de pés é um que é suportada sobre um substrato não-contínua, tal como um anel anular ou aro em oposição a uma pastilha de silício ou lâmina de vidro. Este trabalho descreve um procedimento simples, repetível fabricação de filmes ultrafinos free-standing de polímero que é adequado para filmes de grande-área ou de produção de alto rendimento. É compatível com uma variedade de diferentes polímeros, incluindo o poli (formal de vinilo), poliestireno e poli (metacrilato de metilo). Ele pode ser utilizado para fabricar películas estacionárias que são tão grandes como 13 cm de diâmetro ou tão fino como 10 nm. A fabricação de polímeros free-standing consiste em três etapas básicas: 1) deposition de película de polímero sobre um substrato tradicional tal como uma pastilha ou corrediça, 2) libertação ou descolagem da película a partir do substrato, e 3) de captura da película resultante sobre um suporte. Este artigo detalha um procedimento que consta em um estudo anterior sobre vários métodos de liberação 14. A deposição pode ser conseguida por qualquer número de tecnologias fina película de polímero de base, tais como spin-coating, deposição de vapor, ou de revestimento por imersão. Neste trabalho, nós utilizamos técnicas spin-coating padrão. O &quot;flutuar fora do elevador em&quot; técnica é o método mais comum para a libertação de uma película ultrafina do seu substrato. 15 Nesta técnica, a película e o substrato estão imersos num banho de solvente adequado. O solvente incha o filme e induz a delaminação espontânea, libertando o filme e permitindo-lhe flutuar à superfície do banho. A espessura mínima de filme que podeser lançado usando elevador off-float é determinado pelo equilíbrio entre a energia descamação interfacial com a energia de deformação induzida por inchaço: 16 <img alt="Equação 1" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> (1) Onde L representa a espessura do filme, ν f é relação entre o filme de Poisson, E é o módulo de Young do filme, ξ é a proporção de inchamento do filme, e γ é a energia interfacial da casca. A maneira típica de contornar a limitação imposta pela Equação (1) é para depositar uma camada intermédia entre a película sacrificial e o substrato de deposição. 17-20 Quando esta camada intermédia se dissolve em um banho de solvente, a película é libertada e pode ser capturada num suporte . Um método relacionado é o método sobrecamada de sacrifício, a qual utiliza descamação mecânica do filme sobre uma camada de sacrifício prIOR à dissolução 21. A utilização de materiais sacrificiais tem vários inconvenientes principais. Em primeiro lugar, a adição de um material do processo adicional e passo pode exigir um compromisso entre as condições de fabrico de filme óptimas condições de processamento e o material sacrificial. Em segundo lugar, materiais sacrificiais podem ser difíceis de depósito, sem afectar as propriedades mecânicas ou a pureza da película final de pés. Em terceiro lugar, o processo para a deposição do material sacrificial deve ser optimizado e monitorizados para a qualidade como uma operação na fabricação global película isenta de pé. 14 Neste trabalho, nós descrevemos uma técnica de modificação de superfície que diminui a energia interfacial descamação, permitindo que o elevador off-float sobre a técnica a ser utilizada para filmes ultrafinos. O substrato é modificada pela deposição de uma montagem de auto-limitada, a auto-optimização quase monocamada de o cloreto de policatião polydiallyldiammonium (PDAC). Por causa daa força da ligação entre o policatião e o substrato, esta modificação da superfície é robusta para os passos subsequentes do processo. A natureza auto-limitada e auto-otimização da formação de quase-monocamada requer praticamente zero otimização e é facilmente escalável para grandes áreas. A seguir à remoção, o filme flutua no topo do banho de solvente, onde é capturado sobre um suporte do tipo aro. Apesar de não ser dada muita atenção na literatura existente, neste trabalho vamos descrever técnicas para capturar filmes da grande-área em suportes que reduzem a probabilidade de rasgar ou danificar o filme.

<table><tbody><tr><td>Vinylec E</td><td>SPI</td><td></td><td></td></tr><tr><td>ethyl lactate, &gt;98%, FCC, FG</td><td>Sigma-Aldrich</td><td>W244007-1KG-K</td><td></td></tr><tr><td>4&quot; silicon wafers &amp;lt;100&gt;, Single side polished</td><td>International Wafer Service</td><td></td><td></td></tr><tr><td>sulfuric acid, 98%, ACS reagent grade</td><td>Sigma-Aldrich</td><td>320501-6X500ML</td><td></td></tr><tr><td>hydrogen peroxide, 30%, semiconductor grade</td><td>Sigma-Aldrich</td><td>316989-3.7L</td><td></td></tr><tr><td>isopropanol, ACS grade, 4 L</td><td>Fisher Scientific</td><td>A464-4</td><td></td></tr><tr><td>dichloromethane, ACS grade</td><td>Alfa-Aesar</td><td>22917</td><td></td></tr><tr><td>deionized water, distilled</td><td></td><td></td><td></td></tr><tr><td>PDAC reagent (Sigma-Aldrich 409014)</td><td>Sigma-Aldrich</td><td>409014</td><td></td></tr><tr><td>Spin Coater</td><td>Laurell Technologies&amp;nbsp;</td><td>WS-650-23</td><td></td></tr><tr><td>Barnstead/Thermolyne Super Nuova explosion-proof hot plate&amp;nbsp;</td><td></td><td></td><td></td></tr><tr><td>explosion-proof forced air oven</td><td>VWR&amp;nbsp;</td><td>1330 FMS&amp;nbsp;</td><td></td></tr><tr><td>balance with a range of 1&amp;nbsp;mg to 1,020&amp;nbsp;g</td><td>Mettler Toledo</td><td>MS1003S</td><td></td></tr><tr><td>reflectance spectrometer</td><td>Filmetrics</td><td>F20-UV</td><td></td></tr><tr><td>manipulator consisting of a Klinger tilt stage, a Brinkman rack-and-pinion and a lab jack&amp;nbsp;</td><td></td><td></td><td></td></tr><tr><td>Cutting tool/template, LLNL-built, no drawings</td><td></td><td></td><td></td></tr><tr><td>straight edge, LLNL, no drawings</td><td></td><td></td><td></td></tr><tr><td>Tent hoop, LLNL</td><td></td><td></td><td></td></tr><tr><td>culture dish 190 mm x 100 mm, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>20 ml beaker, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>250 ml beaker, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>1,000 ml beaker, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>60 ml glass vial with plastic stopper&amp;nbsp;</td><td>VWR</td><td></td><td></td></tr><tr><td>Petri dish, 150 mm diameter x2, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>600 ml beaker x2, Pyrex</td><td>VWR</td><td></td><td></td></tr><tr><td>tweezers, stainless steel</td><td></td><td></td><td></td></tr><tr><td>cutting blade</td><td>Exacto</td><td></td><td></td></tr><tr><td>clean room wipes</td><td>Contec&amp;nbsp;</td><td>PNHS-99</td><td></td></tr><tr><td>polyester knit 9/91 IPA/DI water wipes</td><td>Contec&amp;nbsp;</td><td>Prosat&amp;nbsp;</td><td></td></tr><tr><td>Fluoroware wafer trays</td><td>Ted Pella</td><td>1395-40</td><td></td></tr><tr><td>Nylon Micro fiber (camel hair)</td><td></td><td></td><td></td></tr><tr><td>Disposable BD 3-ml plastic syringe</td><td>VWR</td><td></td><td></td></tr><tr><td>0.2 &amp;#956;m Luer-lock PTFE filters</td><td>Acrodisc&amp;nbsp;</td><td></td><td></td></tr><tr><td>0.45 &amp;#956;m Luer-lock PTFE filters</td><td>Acrodisc&amp;nbsp;</td><td></td><td></td></tr></tbody></table>

fabrication of large-area free-standing ultrathin polymer films

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

A Figura 1 mostra um exemplo de uma película fina de polímero livre de pé sobre uma grande área. Este 55 nm de espessura de filme de polivinil formal foi fabricado usando o processo descrito aqui e é montado em um aro de 13 cm de aço de diâmetro. A delaminação ocorre em grandes áreas, sem a introdução de defeitos que conduzem à rotura do filme. Assim, a resistência intrínseca de polyvinylformal podem ser exploradas mesmo para as películas muito finas. A Figura 2 mostra u...

Watch this Scientific Journal Video about Fabrication of Large-area Free-standing Ultrathin Polymer Films at JoVE.com

Fabrication of Large-area Free-standing Ultrathin Polymer Films

We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

Fabricação de grande-área royalty-pé ultrafinos Polymer Films

This procedure describes a method for the fabrication of large-area and ultrathin free-standing polymer films.  Typically, ultrathin films are prepared ...

fabrication-of-large-area-free-standing-ultrathin-polymer-films

Research

JoVE Journal

Chemistry

15.2K visualizações.  Lawrence Livermore National Laboratory. We describe a method for the fabrication of large-area (up to 13 cm diameter) and ultrathin (as thin as 8 nm) polymer films. Instead of using a sacrificial interlayer to delaminate the film from its substrate, we use a self-limiting surface treatment suitable for arbitrarily large areas.

Vídeo: Fabrication of Large-area Free-standing Ultrathin Polymer Films

Micropunching Lithography for Generating Micro- and Submicron-patterns on Polymer Substrates

Conducting polymers have attracted great attention since the discovery of high conductivity in doped polyacetylene in 19771. They offer the advantages of low weight, easy tailoring of properties and a wide spectrum of applications2,3. Due to sensitivity of conducting polymers to environmental conditions (e.g., air, oxygen, moisture, high temperature and chemical solutions), lithographic techniques present significant technical challenges when working with these materials4. For example, current photolithographic methods, such as ultra-violet (UV), are unsuitable for patterning the conducting polymers due to the involvement of wet and/or dry etching processes in these methods. In addition, current micro/nanosystems mainly have a planar form5,6. One layer of structures is built on the top surfaces of another layer of fabricated features. Multiple layers of these structures are stacked together to form numerous devices on a common substrate. The sidewall surfaces of the microstructures have not been used in constructing devices. On the other hand, sidewall patterns could be used, for example, to build 3-D circuits, modify fluidic channels and direct horizontal growth of nanowires and nanotubes.
A macropunching method has been applied in the manufacturing industry to create macropatterns in a sheet metal for over a hundred years. Motivated by this approach, we have developed a micropunching lithography method (MPL) to overcome the obstacles of patterning conducting polymers and generating sidewall patterns. Like the macropunching method, the MPL also includes two operations (Fig. 1): (i) cutting; and (ii) drawing. The "cutting" operation was applied to pattern three conducting polymers4, polypyrrole (PPy), Poly(3,4-ethylenedioxythiophen)-poly(4-styrenesulphonate) (PEDOT) and polyaniline (PANI). It was also employed to create Al microstructures7. The fabricated microstructures of conducting polymers have been used as humidity8, chemical8, and glucose sensors9. Combined microstructures of Al and conducting polymers have been employed to fabricate capacitors and various heterojunctions9,10,11. The "cutting" operation was also applied to generate submicron-patterns, such as 100- and 500-nm-wide PPy lines as well as 100-nm-wide Au wires. The "drawing" operation was employed for two applications: (i) produce Au sidewall patterns on high density polyethylene (HDPE) channels which could be used for building 3D microsystems12,13,14, and (ii) fabricate polydimethylsiloxane (PDMS) micropillars on HDPE substrates to increase the contact angle of the channel15.

A micropunching lithography approach is developed to generate micro- and submicron-patterns on top, sidewall and bottom surfaces of polymer substrates. It overcomes the obstacles of patterning conducting polymers and generating sidewall patterns. This method allows rapid fabrication of multiple features and is free of aggressive chemistry.

Micropunching Litografia de Geração de Micro e submicrométricas-padrões sobre substratos poliméricos

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

Engenharia

Towards Biomimicking Wood: Fabricated Free-standing Films of Nanocellulose, Lignin, and a Synthetic Polycation

Woody materials are comprised of plant cell walls that contain a layered secondary cell wall composed of structural polymers of polysaccharides and lignin. Layer-by-layer (LbL) assembly process which relies on the assembly of oppositely charged molecules from aqueous solutions was used to build a freestanding composite film of isolated wood polymers of lignin and oxidized nanofibril cellulose (NFC). To facilitate the assembly of these negatively charged polymers, a positively charged polyelectrolyte, poly(diallyldimethylammomium chloride) (PDDA), was used as a linking layer to create this simplified model cell wall. The layered adsorption process was studied quantitatively using quartz crystal microbalance with dissipation monitoring (QCM-D) and ellipsometry. The results showed that layer mass/thickness per adsorbed layer increased as a function of total number of layers. The surface coverage of the adsorbed layers was studied with atomic force microscopy (AFM). Complete coverage of the surface with lignin in all the deposition cycles was found for the system, however, surface coverage by NFC increased with the number of layers. The adsorption process was carried out for 250 cycles (500 bilayers) on a cellulose acetate (CA) substrate. Transparent free-standing LBL assembled nanocomposite films were obtained when the CA substrate was later dissolved in acetone. Scanning electron microscopy (SEM) of the fractured cross-sections showed a lamellar structure, and the thickness per adsorption cycle (PDDA-Lignin-PDDA-NC) was estimated to be 17 nm for two different lignin types used in the study. The data indicates a film with highly controlled architecture where nanocellulose and lignin are spatially deposited on the nanoscale (a polymer-polymer nanocomposites), similar to what is observed in the native cell wall.

The objective of this research was to form synthetic plant cell wall tissue using layer-by-layer assembly of nanocellulose fibrils and isolated lignin assembled from dilute aqueous suspensions.&#160; Surface measurement techniques of quartz crystal microbalance and atomic force microscopy were used to monitor the formation of the polymer-polymer nanocomposite material.

Rumo Biomimicking Madeira: Fabricados free-standing Filmes de nanocellulose, lignina, e uma policátion sintético

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

Química

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

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in combination with their outstanding thermal and chemical stability, and low densities. However, their insoluble nature causes problems in their processing since usually applied techniques such as spin coating are not available. Especially for membrane applications, where the processing of CMP as thin films is desirable, the processing problems have hindered their commercial application.
Here we describe the interfacial synthesis of CMP thin films on functionalized substrates via molecular layer-by-layer (l-b-l) synthesis. This process allows the preparation of films with desired thickness and composition and even desired composition gradients.
The use of sacrificial supports allows the preparation of freestanding membranes by dissolution of the support after the synthesis. To handle such ultra-thin freestanding membranes the protection with sacrificial coatings showed great promise, to avoid rupture of the nanomembranes. To transfer the nanomembranes to the desired substrate, the coated membranes are upfloated at the air-liquid interface and then transferred via dip coating.

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

Síntese camada por camada e Transferência de autônomos conjugados microporosas Polymer Nanomembranes

CMP as large surface area materials have attracted growing interest recently, due to their high variability in the incorporation of functional groups in ...

Reactive Vapor Deposition of Conjugated Polymer Films on Arbitrary Substrates

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. Conductive polymers, poly(3,4-ethylenedioxythiophene) (PEDOT) and poly(3,4-propylenedioxythiophene) (PProDOT), and a semiconducting polymer, poly(thieno[3,2-b]thiophene) (PTT), were deposited on unconventional highly-disordered and textured substrates with high surface areas, such as paper, towels and fabrics. This reported deposition chamber is an improvement of previous vapor reactors because our system can accommodate both volatile and nonvolatile monomers, such as 3,4-propylenedioxythiophene and thieno[3,2-b]thiophene. Utilization of both solid and liquid oxidants are also demonstrated. One limitation of this method is that it lacks sophisticated in situ thickness monitors. Polymer coatings made by the commonly used solution-based coating methods, such as spin-coating and surface grafting, are often not uniform or susceptible to mechanical degradation. This reported vapor phase deposition method overcomes those drawbacks and is a strong alternative to common solution-based coating methods. Notably, polymer films coated by the reported method are uniform and conformal on rough surfaces, even at a micrometer scale. This feature allows for future application of vapor deposited polymers in electronics devices on flexible and highly textured substrates.

This paper presents a protocol for reactive vapor deposition of poly(3,4-ethylenedioxythiophene), poly(3,4-propylenedioxythiophene), and poly(thieno[3,2-b]thiophene) films on glass slides and rough substrates, such as textiles and paper.

Depósito de Vapor reativa dos filmes de polímeros conjugados em substratos arbitrários

We demonstrate a method of conformally coating conjugated polymers on arbitrary substrates using a custom-designed, low-pressure reaction chamber. ...

Fabrication of Ultra-thin Color Films with Highly Absorbing Media Using Oblique Angle Deposition

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present an advanced method for fabricating ultra-thin color films with improved characteristics. The proposed process addresses several fabrication issues, including large area processing. Specifically, the protocol describes a process for fabricating ultra-thin color films using an electron beam evaporator for oblique angle deposition of germanium (Ge) and gold (Au) on silicon (Si) substrates.&#160; Film porosity produced by the oblique angle deposition induces color changes in the ultra-thin film. The degree of color change depends on factors such as deposition angle and film thickness. Fabricated samples of the ultra-thin color films showed improved color tunability and color purity. In addition, the measured reflectance of the fabricated samples was converted into chromatic values and analyzed in terms of color. Our ultra-thin film fabricating method is expected to be used for various ultra-thin film applications such as flexible color electrodes, thin film solar cells, and optical filters. Also, the process developed here for analyzing the color of the fabricated samples is broadly useful for studying various color structures.

We present a detailed method for fabricating ultra-thin color films with improved characteristics for optical coatings. The oblique angle deposition technique using an electron beam evaporator allows improved color tunability and purity. Fabricated films of Ge and Au on Si substrates were analyzed by reflectance measurements and color information conversion.

Fabricação de filmes de cor ultra-fino com altamente absorvente Media usando ângulo oblíquo deposição

Ultra-thin film structures have been studied extensively for use as optical coatings, but performance and fabrication challenges remain.&#160; We present ...

Fabricating Reactive Surfaces with Brush-like and Crosslinked Films of Azlactone-Functionalized Block Co-Polymers

In this paper, fabrication methods that generate novel surfaces using the azlactone-based block co-polymer, poly (glycidyl methacrylate)-block-poly (vinyl dimethyl azlactone) (PGMA-b-PVDMA), are presented. Due to the high reactivity of azlactone groups towards amine, thiol, and hydroxyl groups, PGMA-b-PVDMA surfaces can be modified with secondary molecules to create chemically or biologically functionalized interfaces for a variety of applications. Previous reports of patterned PGMA-b-PVDMA interfaces have used traditional top-down patterning techniques that generate non-uniform films and poorly controlled background chemistries. Here, we describe customized patterning techniques that enable precise deposition of highly uniform PGMA-b-PVDMA films in backgrounds that are chemically inert or that have biomolecule-repellent properties. Importantly, these methods are designed to deposit PGMA-b-PVDMA films in a manner that completely preserves azlactone functionality through each processing step. Patterned films show well-controlled thicknesses that correspond to polymer brushes (~90 nm) or to highly crosslinked structures (~1-10 &#956;m). Brush patterns are generated using either the parylene lift-off or interface directed assembly methods described and are useful for precise modulation of overall chemical surface reactivity by adjusting either the PGMA-b-PVDMA pattern density or the length of the VDMA block. In contrast, the thick, crosslinked PGMA-b-PVDMA patterns are obtained using a customized micro-contact printing technique and offer the benefit of higher loading or capture of secondary material due to higher surface area to volume ratios. Detailed experimental steps, critical film characterizations, and trouble-shooting guides for each fabrication method are discussed.

Surface fabrication methods for patterned deposition of nanometer thick brushes or micron thick, crosslinked films of an azlactone block co-polymer are reported. Critical experimental steps, representative results, and limitations of each method are discussed. These methods are useful for creating functional interfaces with tailored physical features and tunable surface reactivity.

Fabricação de superfícies reativas com escova, como filmes de quitosana de polímeros co bloco Azlactone-acrescida e

In this paper, fabrication methods that generate novel surfaces using the azlactone-based block co-polymer, poly (glycidyl methacrylate)-block-poly (vinyl ...

Thin Film Composite Silicon Elastomers for Cell Culture and Skin Applications: Manufacturing and Characterization

In this protocol, we present methods to fabricate thin elastomer composite films for advanced cell culture applications and for the development of skin adhesives. Two different poly-(dimethyl siloxanes) (PDMS and soft skin adhesive (SSA)), have been used for in depth investigation of biological effects and adhesive characteristics. The composite films consist of a flexible backing layer and an adhesive top coating. Both layers have been manufactured by doctor blade application technique. In the present investigation, the adhesive behavior of the composite films has been investigated as a function of the layer thickness or a variation of the Young&#39;s modulus of the top layer. The Young&#39;s modulus of PDMS has been changed by varying the base to crosslinker mixing ratio. In addition, the thickness of SSA films has been varied from approx. 16 &#181;m to approx. 320 &#181;m. Scanning electron microscopy (SEM) and optical microscopy have been used for thickness measurements. The adhesive properties of elastomer films depend strongly on the film thickness, the Young&#39;s modulus of the polymers and surface characteristics. Therefore, normal adhesion of these films on glass substrates exhibiting smooth and rough surfaces has been investigated. Pull-off stress and work of separation are dependent on the mixing ratio of silicone elastomers.
Additionally, the thickness of the soft skin adhesive placed on top of a supportive backing layer has been varied in order to produce patches for skin applications. Cytotoxicity, proliferation and cellular adhesion of L929 murine fibroblasts on PDMS films (mixing ratio 10:1) and SSA films (mixing ratio 50:50) have been conducted. We have shown here, for the first time, the side by side comparison of thin composite films manufactured of both polymers and present the investigation of their biological- and adhesive properties.

A protocol for the manufacturing process of polymeric thin film composite structures possessing either different Young&#39;s moduli or thicknesses is presented. Films are produced for advanced cell culture studies or as skin adhesives.

Fina película composta de silício elastômeros para aplicações de pele e cultura de pilha: fabricação e caracterização

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

Biologia do Desenvolvimento

Procedure for the Transfer of Polymer Films Onto Porous Substrates with Minimized Defects

The fabrication of devices containing thin film composite membranes necessitates the transfer of these films onto the surfaces of arbitrary support substrates. Accomplishing this transfer in a highly controlled, mechanized, and reproducible manner can eliminate the creation of macroscale defect structures (e.g., tears, cracks, and wrinkles) within the thin film that compromise device performance and the usable area per sample. Here, we describe a general protocol for the highly controlled and mechanized transfer of a polymeric thin film onto an arbitrary porous support substrate for eventual use as a water filtration membrane device. Specifically, we fabricate a block copolymer (BCP) thin film on top of a sacrificial, water-soluble poly(acrylic acid) (PAA) layer and silicon wafer substrate. We then utilize a custom-designed, 3D-printed transfer tool and drain chamber system to deposit, lift-off, and transfer the BCP thin film onto the center of a porous anodized aluminum oxide (AAO) support disc. The transferred BCP thin film is shown to be consistently placed onto the center of the support surface due to the guidance of the meniscus formed between the water and the 3D-printed plastic drain chamber. We also compare our mechanized transfer-processed thin films to those that have been transferred by hand with the use of tweezers. Optical inspection and image analysis of the transferred thin films from the mechanized process confirm that little-to-no macroscale inhomogeneities or plastic deformations are produced, as compared to the multitude of tears and wrinkles produced from manual transfer by hand. Our results suggest that the proposed strategy for thin film transfer can reduce defects when compared to other methods across many systems and applications.

We present a procedure for highly controlled and wrinkle-free transfer of block copolymer thin films onto porous support substrates using a 3D-printed drain chamber. The drain chamber design is of general relevance to all procedures involving transfer of macromolecular films onto porous substrates, which is normally done by hand in an irreproducible fashion.

Procedimento para transferência de películas de polímero para substratos porosos com defeitos minimizados

The fabrication of devices containing thin film composite membranes necessitates the transfer of these films onto the surfaces of arbitrary support ...

A Femtoliter Droplet Array for Massively Parallel Protein Synthesis from Single DNA Molecules

Advances in spatial resolution and detection sensitivity of scientific instrumentation make it possible to apply small reactors for biological and chemical research. To meet the demand for high-performance microreactors, we developed a femtoliter droplet array (FemDA) device and exemplified its application in massively parallel cell-free protein synthesis (CFPS) reactions. Over one million uniform droplets were readily generated within a finger-sized area using a two-step oil-sealing protocol. Every droplet was anchored in a femtoliter microchamber composed of a hydrophilic bottom and a hydrophobic sidewall. The hybrid hydrophilic-in-hydrophobic structure and the dedicated sealing oils and surfactants are crucial for stably retaining the femtoliter aqueous solution in the femtoliter space without evaporation loss. The femtoliter configuration and the simple structure of the FemDA device allowed minimal reagent consumption. The uniform dimension of the droplet reactors made large-scale quantitative and time-course measurements convincing and reliable. The FemDA technology correlated the protein yield of the CFPS reaction with the number of DNA molecules in each droplet. We streamlined the procedures about the microfabrication of the device, the formation of the femtoliter droplets, and the acquisition and analysis of the microscopic image data. The detailed protocol with the optimized low running cost makes the FemDA technology accessible to everyone who has standard cleanroom facilities and a conventional fluorescence microscope in their own place.

The overall goal of the protocol is to prepare over one million ordered, uniform, stable, and biocompatible femtoliter droplets on a 1 cm2 planar substrate that can be used for cell-free protein synthesis.

Uma matriz de gotícula femtoliter para síntese de proteínas massivamente paralelas de moléculas de DNA único

Advances in spatial resolution and detection sensitivity of scientific instrumentation make it possible to apply small reactors for biological and ...

A Simple and Scalable Fabrication Method for Organic Electronic Devices on Textiles

Today, wearable electronics devices combine a large variety of functional, stretchable, and flexible technologies. However, in many cases, these devices cannot be worn under everyday conditions. Therefore, textiles are commonly considered the best substrate to accommodate electronic devices in wearable use. In this paper, we describe how to selectively pattern organic electroactive materials on textiles from a solution in an easy and scalable manner. This versatile deposition technique enables the fabrication of wearable organic electronic devices on clothes.

In this paper, we present a protocol to selectively deposit organic materials on textiles, which allows for the direct integration of organic electronic devices with wearables. The fabricated devices can be fully integrated in textiles, respecting their mechanical appearance and enabling sensing capabilities.

Um método de fabricação simples e escalável para dispositivos eletrônicos orgânicos sobre os têxteis

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