Sözleşme DE-AC52-07NA27344 altında Lawrence Livermore Ulusal Laboratuvarı tarafından ABD Enerji Bakanlığı himayesinde gerçekleştirilen bu çalışma.

1. Çözelti Hazırlama <ol><li> Bir şırınga ve bir 0.20 um şırınga filtresi kullanılarak etil laktat 60 g filtre. Etil laktat resmi polivinil 0.3 g ekleyin. 4 saat 50 ° C de fırın içine çözelti yerleştirin. Polimer tamamen çözülene olup olmadığını görmek için hafifçe sallayın flakon. <ol><li> Çözüm bulutlu ya da hala optik homojen olmayan düzensizlikleri gösteriyorsa, başka bir 2 saat boyunca fırına flakon dönün. Bu tarif, tipik olarak film kalınlıkları yaklaşık 30 nm için kullanılan bir% 0.5 ağırlık polimer çözeltisi, içindir. Daha yüksek bir polimer, ağırlık olarak içeriği ile çözüm daha kalın filmler için kullanılabilir. </li></ol></li><li> 20 ml&#39;lik bir volumetrik şişe içine PDAC reajanı 1,0 g ağırlığındaki ve deiyonize (Dİ) su ile ölçüm hattına balon doldurarak PDAC çözelti hazırlayın. Yumuşak bir depolama kabına aktarmadan önce çözelti döndürülür. </li></ol> 2. Yüzey Hazırlığı <ol><li> DİKKAT. Konsantre edilmiş sülfürik 60 ml dökünTemiz bir 250 ml&#39;lik bir deney şişesine asit elde edildi. Yavaş yavaş% 30 hidrojen peroksit 20 ml ekleyin. Geçene dumanlı, yavaşça çözüm girdap kadar bekleyin. çözüm ve beher çok sıcak olacak ve karışım korozif değildir. </li><li> Sıcak plaka üzerine 150 mm Petri kabı yerleştirin ve çanak içine asit dökün. 100 ° C&#39;ye kadar sıcak plaka ayarlayın. <ol><li> Cilalı yüzü yukarı bakacak şekilde aside 4 &#39;silikon gofret yerleştirin. Yavaşça tüm yüzey ıslatılır emin olmak için bir cımbız ile ortada gofret bastırın. 30 dakika boyunca asit içinde gofret bırakın. </li></ol></li><li> Bir cımbız ile asitten gofret çıkarın ve ön durulama ve arka gofret iyice DI su ile fışkırtma şişeden. Su düzenli bir desen levha kapalı olmalıdır. Temiz bir tezgah gofret kurutun. </li><li> Filtre montaj şırınga içine sıvı çizerek PDAC solüsyonu ile atılabilir bir 3 ml&#39;lik şırınga ve DI suyla önce 0.2 mikron filtre ve durulayın ven filtre aracılığıyla sıvıyı dışarı iterek. </li><li> Spin kaplayıcı bir temizlenmiş gofret monte edin. Şırıngaya PDAC çözümünün kadar 1.0-1.2 ml çizin ve gofret ortasında üzerine filtre olsa dağıtmak. 15 sn için 4000 rpm&#39;de döndürün, daha sonra (50 ° C&#39;ye önceden ısıtılmış) sıcak bir plaka gofret aktarmak ve 30 saniye boyunca bekletin. </li><li> DI su ile kurutulmuş PDAC katmanı durulayın ve temiz tezgah gofret kurumaya bırakın. </li></ol> 3. Film İmalatı <ol><li> Savurmalı kaplayıcının üzerine kuru PDAC ile muamele gofret yerleştirin. </li><li> Tek kullanımlık bir 3 ml&#39;lik şırınga ve 2.4&#39;de prosedür kullanılarak etil laktat çözelti) bir 0.45 mikron filtre durulayın. </li><li> Deposit sonra 200 rpm&#39;de 10 saniye boyunca gofret ve spin ortasında şırınga ile filtre boyunca etil laktat çözeltisi 2.5 mi, 1,700 rpm&#39;de (arzu edilen film kalınlığına bağlı olarak), 3 sn. Gofret üzerinde üniform bir sıvı filmi olmalıdır. </li><li> Spin kaplayıcı film kurumasını bekleyinBu (tipik olarak 10-15 dakika) gözle görülür kuruyana kadar, daha sonra 10 dakika boyunca (50 ° C&#39;ye kadar ısıtılır) bir sıcak plaka üzerine yerleştirin. </li><li> , Liftoff için tipik olarak 2 cm x 2 cm küçük kareler halinde filmler zar, fakat kullanılan film yuvasına (3.5.1-3.5.2) boyutuna bağlı olarak, daha büyük olabilir. Alternatif olarak, bir gofret boyutlu filmi (3.5.3) delaminating için iki din bilginleri yapmak. Not: Standart filmin sahipleri ortasında 13 mm çapında bir dairesel açıklık ile, 19 x 19 mm&#39;dir. Gofret boyutlu filmler için, &quot;çok ince bisküviden daha küçük 1 olan bir çapa sahip bir tel çember (bir daire haline getirilebilir, örneğin, paslanmaz çelik tel) kullanın. Filmler tipik olarak liftoff ve kabarma sırasında su absorbe çünkü bir dairesel açıklık seçilir. Filmler tutucu kurumasına gibi, su çıkarılır ve film küçülecek. Bir dairesel açıklık stresin eşit dağılım sağlar. <ol><li> Bir kesim şablonu üzerinde gofret yerleştirin. Düz e önlemek için tüm kenarları gofret daha uzun boylu olduğu bir kare şablon kullanındge gofret dokunmadan lıklar sırasında bıçak yönlendirmek için kullanılır. Dicing sırasında düz kenar yerleştirme rehberlik 2 cm aralıklarla kenarları işaretleyin. Hizalamak için iki kenarlarına gofret itin. </li><li> İki hizalama işaretleri boyunca bir cetvel yerleştirin ve filmi çizmek için düz kenarı boyunca yavaşça jilet çizin. Filmi işaretlemek için yeterli basınç uygulayın, ama çok fazla değil gofret kendisi işaretlemek ve parçacıkları üretmek. Kalın filmlerde, kesme hattı açıkça görülebilir olacak. </li><li> Gofret tek parça halinde bir film Fırlatmaya, bir jilet ile gofret kenar açıklanacaktır. Gofret iki daireden arasında rack-and-pinyon üzerine gofret kelepçe yeterince geniş bir şerit işaretleyiniz. </li></ol></li><li> DI su ile 190 x 100 mm kültür çanak doldurun. Bir eğim aşamasına monte edilmiş bir rack-and-pinyona büyük düz gofretin Kelepçe ve yavaş yavaş DI suya indirin. Film suyu hattında gofret ayrılması gerekir. <ol><li> WAF düşürücü Devamyerine su hattı altında havalanma arayüzü iterek yerine, gofret ayırmak için filmin yeterince zaman verir bir oranda er. Kareler ilk satırı gofret müstakil ve yüzeyinde yüzen olduğunda, gofret düşürücü duraklatmak. Film tamamen ayrılana kadar bir gofret boyutlu film için, gofret çeker devam edin. </li><li> Suya Film sahibinin başını daldırın ve film altına taşıyın. Film kenarlarından biri çember kolu kenarını sıraya ve film ile çember dokunmayın. Eğer başarılı olursa, film, hoop sadık olacaktır. <ol><li> Bir gofret boyutlu film için, kenardan uzak tarif bölümünün altında tel çember, sadece bir santimetre yerleştirin. Çember, yakalama başlayan film, çember etrafında sarın ve kendi üzerine geri katlayın, böylece filmin kenarı ve çember kenarı arasındaki bazı mesafeyi muhafaza önce filmin altında merkezli olduğundan emin olun. </li></ol></li><li> Bir su yavaşça çember geri çekin35 ° &#39;lik açısı. Çok yavaş sudan dışarı filmi kaldırın. Not: Filmin yaklaşık yarısı (su yüzeyine, yani normal) yaklaşık 90 ° sudan çekilmesinden sonra en az 20 nm kalınlığında filmler için, tutucu boyunca filmin çekme önlemek için açı artar. Asansör dışarı açısını değiştirirken, çember üzerinden filmin çekerek önlemek için çok yavaş yapın. </li><li> Çember tamamen geri çekildiğinde, kuruması için bir kenara koyun. Emin çember alt aşağı çember koymadan önce damla ücretsiz olun ve çember ile yüzey arasında bir sıvı mühür yaratmaktan kaçınmak için (örneğin bir gofret tepsi gibi) bir eğri yüzey kullanın. </li><li> Daha fazla kayıtsız kalamayız kareler gofret kalırsa, suya gofret düşürücü devam edip adımları tekrarlayın 3.6.1-3.6.4 yukarıda kalan kareler için. </li><li> Filmlere kuru O / N edelim. </li></ol></li></ol>

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Yazarlar ifşa hiçbir şey yok.

PDAC substrat tedavisi. Kolaylıkla olumsuz (örneğin, silikon veya cam) tahsil kaydıyla tedavi edilen veya herhangi bir boyutta substratlar, yani kendini sınırlayan elektrostatik etkileşimler dayalı 1-2 13 cm&#39;ye kadar çok büyük ince filmler (gösterir Figures edilir çapında) tek değişiklik kullanılan reaktiflerin hacmi olmak, bu protokolü kullanarak imal. Nihai elde boyutu sadece kaplama ve delaminasyon cihazları veya serbest duran yapı imal etmek için ku...

Serbest duran ince polimer filmleri 5-8. Sensörler, 1-3 MEMS&#39;ler katalizi ya da süzme, 4 ve doku mühendisliği de dahil olmak üzere çeşitli uygulamalarda kullanılır Ayrıca kapalı alan içinde polimer davranışının keşfetmek temel çalışmaları için kullanılır. 9- 13 Bir serbest duran bir film gibi halka şeklinde bir halka veya bir silikon veya cam slayt karşı çember olarak kesintili bir alt-tabaka üzerinde desteklenmiştir biridir. Bu çalışma, büyük alanlı filmler ya da yüksek verimli üretimi için uygun olan ultra ince serbest duran polimer filmler için basit, tekrar üretim işlemini tarif etmektedir. Bu poli (vinil formal), polistiren ve poli (metil metakrilat) gibi farklı polimerlerin çeşitli ile uyumludur. Bu 13 cm çap kadar büyük ya da 10 nm kadar ince serbest duran filmler imal etmek için de kullanılabilir. serbest duran polimerlerin imalatı üç temel aşamadan oluşmaktadır: 1) dgeleneksel bir alt-tabaka üzerine polimer filmin eposition bir destek üzerine bir gofret veya saydam, 2) serbest bırakılması ya da alt-tabaka filmin liftoff ve elde edilen film 3) yakalama gibi. Bu yazıda çeşitli bırakma yöntemleri konusunda daha önceki bir çalışmada bildirilen bir prosedürü göstermektedir. 14 Biriktirme gibi spin kaplama, buhar biriktirme veya daldırmalı kaplama gibi temel polimer ince film teknolojisi herhangi bir sayıda elde edilebilir. Bu çalışmada, standart spin-kaplama teknikleri kullanmaktadır. Tekniği &quot;lift dışı float&quot;, uygun bir solvent banyosuna daldırılır Bu teknik, film ve alt-tabaka olarak en yaygın olarak alt-tabaka arasında bir çok ince bir film bırakmak için bir yöntem. 15&#39;dir. Solvent, film şişen ve filmin serbest ve banyo içerisinde en üstünde yüzmesini sağlayan kendiliğinden delaminasyona yol açmaktadır. minimum film kalınlığı canasansör kullanarak yayımladı edilmesi off-şamandıra şişme kaynaklı gerilme enerjisi ile arayüzey soyma enerjisini dengelemek suretiyle belirlenir tarih: 16 <img alt="Denklem 1" src="/files/ftp_upload/52832/52832eq1.jpg" width="200" /> (1) L film kalınlığı olduğunda, ν f filmin Poisson oranı, E filmin Young modülü olup, ξ filmin şişme oranı ve γ soyulması ara yüzey enerjisidir. Denklem tarafından uygulanan sınırlama atlamak için tipik bir şekilde (1) film ve alt-tabaka arasında bir yerleştirme geçici ara tabaka yatırmak için. 17-20, bu ara tabaka, bir solvent banyosuna çözündüğü zaman, filmin serbest bırakılır ve bir destek üzerinde yakalanabilir . İlgili bir yöntem kurban katman pr üzerine filmin mekanik soyma kullanır kurban üstteki tabaka yöntemidirdağılmasına IOR. 21 kurbanlık malzemelerin kullanımı birkaç baş sakıncaları vardır. İlk olarak, bir ilave işlemi malzeme ve adım eklenmesi uygun bir film üretim koşulları ve geçici malzemenin işlem koşulları arasında bir uzlaşma gerektirebilir. İkincisi, kurbanlık malzemeler nihai serbest duran filmin mekanik özelliklerini veya saflığını etkilemeden mevduat zor olabilir. Üçüncüsü, kurbanlık malzeme yatırma işlemi optimize edilmiş ve genel serbest duran bir film üretiminde bir operasyon olarak kalite açısından takip edilmelidir. 14 Bu çalışmada, ultra ince filmler için kullanılacak off-şamandıra tekniği asansör sağlayarak, arayüzey soyma enerjisini azaltan bir yüzey modifikasyonu tekniğini açıklar. yerleştirme alt-tabaka polikatyon polydiallyldiammonium klorür (PDAC) içindeki bir kendi kendini sınırlayan, kendinden optimize yakın tek tabaka monte edilmesiyle modifiye edilir. Nedeniylepolikatyon ve alt-tabaka arasındaki bağlanmanın kuvveti, bu yüzey modifikasyonu takip eden işlem adımlarına sağlamdır. yakın tek tabaka oluşumu kendini sınırlayan ve kendini optimize doğa hemen hemen sıfır optimizasyon gerektirir ve geniş alanlara kolayca ölçeklenebilir. Çıkarıldıktan sonra, film, bir çember gibi bir destek üzerinde yakalanır solvent banyosuna üst kısmında yüzen. Kaybolmamış literatüründe çok dikkat verilmez iken, bu çalışmada biz sulanma veya başka filmin zarar olasılığını azaltmak destekte geniş alan filmleri yakalamak için teknikler anlatacağız.

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

fabrication of large-area free-standing ultrathin polymer films

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

Şekil 1, geniş bir alan üzerinde bir serbest-duran ince bir polimer filmin bir örneği göstermektedir. Bu 55 nm kalınlığında polivinil resmi filmi prosedürü burada açıklanan ve 13 cm çapında çelik çember üzerine monte edilmiştir kullanılarak imal edilmiştir. delaminasyon filmin yırtılmaya yol kusurları tanıtan olmadan büyük alanlar üzerinde gerçekleşir. Böylece, polivinilformal içsel gücü çok ince filmler için bile kullanılabilir. Şekil 2 ve&gt; 3x1...

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.

Geniş alanlı Fabrikasyon Ultrathin Polimer Filmler Serbest ayakta

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

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

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

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

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

Nanocellulose, Lignin Fabrikasyon Serbest duran Filmler ve Sentetik polikatiyon: Biomimicking Wood Doğru

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

Kimya

Confocal Imaging of Confined Quiescent and Flowing Colloid-polymer Mixtures

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

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

Kuşatılmış Quiescent ve akan Koloidno polimer Karışımlarının Eşodaklı Görüntüleme

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

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

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

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

Phosphopeptides Gelişmiş Zenginleştirme için Makrogözenekli Polimer Monoliths üzerinde yüksek Gözenekli Koordinasyon Polymer Coatings Hazırlanması

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

Photodynamic Therapy with Blended Conducting Polymer/Fullerene Nanoparticle Photosensitizers

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

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

Karma Polimer / Fulleren Nanopartikül photosensitizers Şefliği ile Fotodinamik Tedavi

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

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

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

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

Puan Bağımlı Elipsometri Ölçümleri Soğutma İnce Camsı Filmlerin dinamikleri belirleme

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

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

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

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

Termo-tersinir Çapraz bağlı Lastik Via Diels-Alder Kimya hazırlanması ve Özellikleri

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

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

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

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

Kapiler Elektroforez Real Time Kitosan Films üzerine Peptit Aşılama Monitör

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

Fabrication and Testing of Photonic Thermometers

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

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

İmalat ve fotonik termometreler test

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

Microfluidic Dry-spinning and Characterization of Regenerated Silk Fibroin Fibers

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

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

Mikrosıvısal kuru-iplik ve rejenere ipek Fibroin lifleri karakterizasyonu

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

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

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

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

Zaman karar vermek Photophysical karakterizasyonu üçlüsü-hasat organik bileşikler bir oksijensiz ortamı kullanarak bir ICCD kamera

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