Biz Advanced Materials için Zernike Enstitüsü, Groningen Üniversitesi tarafından mali destek kabul.

Çift Gyroid Morfoloji 1. Hazırlanması ve PS-b-P4VP karakterizasyonu (PDP) Kompleksleri <ol><li> Tartılır polistiren-blok-poli (4-vinilpiridin) (PS-b-P4VP) ve pentadesilfenol (PDP, E r = 304,51 g / mol.) Olmalıdır gyroid morfolojisi elde etmek için dikkatlice PDP miktarını seçmek ((P4VP (PDP) f) ca olmalıdır P4VP (PDP) bloğun ağırlık fraksiyonu. 0,6 doğrusal AB diblok kopolimerlerin faz diyagramına göre). Genellikle, PS-b-P4VP of 0,15-0,2 g (adım 1.3 &#39;de kullanılan bir Petri kabı çapı 5-6 cm olduğu göz önüne alındığında) PS-b-P4VP 50-100 mikron kalınlığında (PDP) filmler yol açar. Aşağıdaki denklemlere göre PDP miktarını hesaplayın: <img alt="Denklem 1" src="/files/ftp_upload/50673/50673eq1.jpg" /> <img alt="Denklem 2" src="/files/ftp_upload/50673/50673eq2.jpg" /> <img alt="Denklem 3" src="/files/ftp_upload/50673/50673eq3.jpg" /><br/&gt; <img alt="Denklem 4" src="/files/ftp_upload/50673/50673eq4.jpg" /></li><li> Kloroform içinde PS-b-P4VP ve PDP çözülür ve oda sıcaklığında bir kaç saat için karıştırılmıştır. Homojen kompleks oluşumunu sağlamak için ağırlıkça% 2 altında polimer konsantrasyonunu korumak. </li><li> Cam bir Petri kabı içine çözüm dökün. </li><li> Doymuş kloroform atmosfere çanak yerleştirin. </li><li> Yaklaşık bir hafta sonra, Petri kabı çıkarın. Supramoleküler kompleks bir film oluşturulur. </li><li> Gece boyunca 30 ° C&#39;de vakum içinde film kurutun. </li><li> Özel olarak tasarlanmış bir kap içinde film yerleştirin, kaptan havayı çıkarmak ve daha sonra nitrojen ile doldurun. 1 bar basınçta N2 atmosferi altında 120 ° C de fırın içinde 4 gün için filmin tavlanması. </li><li> Epoksi gömmek filmin küçük bir parça, kesme ve 40 ° C&#39;de gece boyunca onu tedavi </li><li> Oda sıcaklığında bir elmas bıçak kullanılarak yaklaşık 80 nm&#39;lik bir kalınlığa örnek mikrotom. ThE mikrotome bölümü su üstünde yüzer. Onları almak ve Cu ızgaraların üzerine yerleştirin. </li><li> Iyot ile bir kavanoza mikrotome bölümleri içeren ızgaraları koydu. 45 dk örnekleri lekeli ve transmisyon elektron mikroskobu için hazırız sonra. </li><li> 120 kV ve görüntü numunenin bir hızlandırma voltajında ​​çalışma transmisyon elektron mikroskobunda lekeli bölümleri ile Cu ızgaraları yerleştirin. </li><li> Küçük açılı X-ışını dağılımı için numune tutucuya (adım 1.7 sonra elde edilen), filmin bir parçası yerleştirin ve bir Kapton bantla sabitleyin. SAXS için makinenin içine hazırlanan numune tutucu yerleştirin. X-ışını deklanşörü açın ve 2D saçılma deseni kazanır. Elde edilen 2 boyutlu desen entegre ve 1D model içindeki yükseltilerin konumunu analiz eder. </li></ol> Gözenekli Yapı 2.. Üretilmesi ve karakterizasyonu <ol><li> Etanol (adım 1.7 sonra elde edilen), filmin bir parçası koyun ve üç gün için muhafaza edin. </li><li> Örnek kurutun. </li><li> Ön1H NMR ölçümler için numune hazırlayın. PDP tozu, PS-b-P4VP tozu, CDCI3 (adım 2.2 sonra) supramoleküler kompleks PS-b-P4VP (PDP) (adım 1.7 sonra) ve gözenekli bir film içinde çözündürülür. Oda sıcaklığında kayıt 1H NMR spektrumu. </li><li> PS-b-P4VP tozu analiz, çok moleküllü kompleks PS-b-P4VP (PDP) (adım 1.7 sonra) ve diferansiyel tarama kalorimetresi ile, gözenekli bir film (adım 2.2 sonra). 1 ° C / dk &#39;lık bir ısıtma / soğutma hızıyla, 0.5 ° C&#39;lik bir titreşim genliği, 60 sn&#39; lik bir salınım süresi ile modüle edilmiş bir modu kullanın. -30 ° C&#39;de dengeye örnekleri, ısı 180 ° C, -30 ° C&#39;ye soğutun ve sonra da 180 ° yeniden ısıtmak C. Analiz için, ikinci ısıtma döngüsünden verileri kullanın. </li><li> 70 ° C&#39;de, oda sıcaklığında 8 saat ve 18 saat için (adım 2.2) sonra gözenekli numune gazın atılması ve 77 K nitrojen adsorpsiyonu ölçümler yapmak </li><li> Uygun yazılımı (örneğin, WinAD kullanınP) ve elde edilen izotermleri analiz modelleri. </li><li> 2 saat boyunca 0.5 Pa arasında, oda sıcaklığında ve basıncında 8 saat ve gaz çıkışına da 50 ° C &#39;de (adım 2.2) sonra gözenekli örnek kurutun. </li><li> Cıva porosimetrisi gerçekleştirin. </li></ol> Polimer Şablon 3. Ekleme Nikel <ol><li> Kalay klorid (SnCl2, E r = 189.60 g / mol) tartılır ve bir sulu solüsyonu (0.1 M SnCl2 / 0.1 M HCI, 1.896 g SnCl2, 0.8 ml HCl ve 100 ml 2 H O) hazırlar. SnCI2 tam olarak çözünmesini sağlamak için, bir çalkalayıcı üzerinde gece boyunca çözelti koyun. </li><li> Palladyum klorid (PdCl2, E r = 177,33 g / mol) tartılır ve bir sulu solüsyonu (0.0014 M PdCl2 / 0.25 M HCl, 0.025 g PdCl2, 2 ml HCl ve 100 ml 2 H O) hazırlar. </li><li> Nikel kaplama banyosunda parçası 1 hazırlayın: Çıkış 6.78 g nikel sülfat hegzahidratı tartmak (Niso 4 • 6H 2 O, M r = 2620,85 g / mol) ve 2 g sodyum sitrat (Na 3 C6 H 5 O 7, E r = 258,06 g / mol) ve 80 ml ​​su bunları çözülür. 828 ul% 85 laktik asit (C3 H 6 O 3, E r = 90,08 g / mol) ilave edin. </li><li> Nikel kaplama banyosunun hazırlanması parçası 2: ağırlık üzerinden 0.2 g dimetilamin boran kompleksi ((CH3) 2 NHBH 3, E r = 58,92 g / mol) ve 20 ml su içinde çözülür. Boran dimetilamindir karmaşık iyi havalandırılan bir davlumbaz ele alınmalıdır. </li><li> 1 saat boyunca kalay klorür (adım 3.1) sulu çözelti içinde, gözenekli filmi (adım 2.2 sonra) bırakın. </li><li> Iyonu giderilmiş su ile iyice yıkayın filmi. </li><li> 1 saat boyunca palladyum klorür (adım 3.2) sulu çözelti içinde film bırakın. </li><li> Iyonu giderilmiş su ile iyice yıkayın filmi. </li><li> Bölüm 1 (3.3) ve nikel kaplama banyosunun parçası 2 (3.4) karıştırın. Amonyum hidroksit kullanılarak pH 7.0 &#39;a ayarlayın. </li><li> 1 saat için, nikel kaplama banyosu içinde film bırakın. </li><li> Iyonu giderilmiş su ile iyice yıkayın filmi. </li><li> Örnek kurutun. </li><li> 1.8-1.9 adımda tarif edildiği gibi elektron mikroskobu için kaplama örnek hazırlayın. </li><li> Resim aşama 1.11 tarif edildiği gibi örnek. </li><li> Yüksek çözünürlüklü transmisyon elektron mikroskobunda kaplama numunenin bölümlerini içeren Cu ızgaraları yerleştirin. Yüksek çözünürlüklü TEM mikrografikleri edinin. Mikroskop altında örnek gözlemlemek ve EDX (X-ışınlarının Enerji Dağılım Analizi) element analizi için alanı seçin. Seçilen alanın EDX analizi gerçekleştirmek ve elde edilen desen analiz. </li></ol> Ters Gyroid Nikel Köpük 4. Pozlama <ol><li> 350 ° C&#39;de bir fırında nikel kaplama filmi (adım 3.12 sonra) koyun ve 4 gün için 1 saat kadar onu tutmak. </li><li> Bir gümüş macun kullanılarak numune tutucu için örnek takın. </li><li> Taramalı elektron mikrofon içine örnek yerleştirinroscope. Numunenin birkaç görüntü kazanır. </li><li> Tarama elektron mikroskobu içine örnek yerleştirin. Mikroskop altında örnek gözlemlemek ve EDX elemental analiz için alanı seçin. Seçilen alanın EDX analizi gerçekleştirmek ve elde edilen desen analiz. </li></ol>

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M., Wiesner, U. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+plumber's+nightmare:+a+new+morphology+in+block+copolymer-ceramic+nanocomposites+and+mesoporous+aluminosilicates.">The plumber's nightmare: a new morphology in block copolymer-ceramic nanocomposites and mesoporous aluminosilicates.</a> J. Am. Chem. Soc. 125, 13084-13093 (2003).</li><li>Tyler, C. A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Orthorhombic+Fddd+network+in+triblock+and+diblock+copolymer+melts.">Orthorhombic Fddd network in triblock and diblock copolymer melts.</a> Phys. Rev. Lett. 94, 208-302 (2005).</li><li>Ranjan, A., Morse, D. C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Landau+theory+of+the+orthorhombic+Fddd+phase.">Landau theory of the orthorhombic Fddd phase.</a> Phys. Rev. E. 74, 011803 (2006).</li><li>Kim, M. I., 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=Stability+of+the+Fddd+Phase+in+Diblock+Copolymer+Melts.">Stability of the Fddd Phase in Diblock Copolymer Melts.</a> Macromolecules. 41, 7667-7670 (2008).</li></ol>

Yazarlar herhangi bir mali çıkarlarını beyan.

Supramolecular kompleksleri başarıyla iyi sıralı metal nanofoams öncüleri olarak uygulanır. Bu yöntemde, önemli bir adım gyroid morfolojisi olan bir şablon, yani, uygun şablon elde etmektir. Blok kopolimerlerin faz diyagramında gyroid bölge çok küçüktür ve bu hedef için oldukça zordur. Bu, geleneksel blok kopolimerleri, başlangıç ​​maddeleri olarak kullanıldığında, oldukça ayrıntılı sentez gyroid morfolojiye yol açar, istenen bileşim, ulaşılana kadar tekrar edilmesi anlam...

Metal nanofoams hazırlanması için mevcut çeşitli teknikler vardır: 1-3 Bozunumu, sol-jel, 6,7 nanosmelting, 4,5 yaklaşımları ve yanma sentezi 8. Bozunumu işleminde, başlangıç ​​malzemesi, genellikle, örneğin bir ikili alaşım, gümüş ve altın bir alaşımdır. Daha az soy metal, bu durumda, gümüş, ya kimyasal ya da elektro-kimyasal bağ ile nano boyutlu bir düzensiz altın gözenekli bir köpük elde kaldırılabilir. Yanma sentezde, metal ile ayrışma sırasında enerjiyi serbest bırakır ve metal nanofoam 8 oluşumunu tahrik enerjik bir öncüsü ile karıştırılır. Metal köpüklerin mekanik davranışı ile ilgili çalışmalar düzensiz mimarilerinde gerilmeler genel makro-9-11 bağ nano itibaren etkili bir şekilde iletilmesini edilemez olduğunu göstermektedir. Böylece iyi sıralı metal nanofoams ile karşılaştırıldığında, üstün mekanik özelliklere sahip olmaları beklenmektedirdüzensiz olanlar. Burada temsil Fikir metal nanofoams için ön-maddeler olarak sipariş Nano halinde kendi kendine birleşebilen blok kopolimerleri kullanmaktır. Küresel, silindirik, ince tabakalı, çift gyroid, altıgen delikli lameller, ve diğerleri 12-14: bir blok kopolimer, monomer birimlerinin toplam sayısı ve kimyasal olarak bağlı olan bloklar arasındaki itme ölçüde bileşimine bağlı olarak, çeşitli morfolojileri gibi görünür . Bundan başka, polimer blokları nano gözenekli malzeme 15 yol seçici olarak parçalanabilir. En yaygın yöntemler şunlardır: ozon ayrışımını 16-18, UV ışınlaması 19, reaktif iyon aşındırma 20-22, 23-26 ve çözünme. Oluşturulan gözenekli yapılar, çeşitli inorganik malzemeler ile geri dolduruldu edilebilir. Metal oksitler (örneğin, SiO 2, TiO 2), genellikle şablonunun kanal içine 27-29, sol-jel yöntemi ile tanıtılmaktadır. Electrochemical ve elektriksiz kaplama genellikle 30-33 içine veya şablonlar üzerine metal yatırmak için kullanılır. Son olarak, kalan polimer vb piroliz 2, çözünme 34,35, 28,29 UV bozulması vasıtasıyla polimer / inorganik nanohibrit kaldırılabilir Bizim bir yaklaşım olarak, polistiren-blok-poli (4-vinilpiridin) bir supramoleküler kompleksi (PS-b-P4VP) iki bloklu kopolimer ve amfifilik pentadesilfenol (PDP) molekülleri başlar. Bu kompleks PDP ve piridin halkaları (Şekil 1a) arasındaki hidrojen bağı bir sonucudur. Başlangıç ​​blok kopolimerin bileşimi ve ilave PDP miktarı öyle bir şekilde seçilir ki, bir ağ ve bir PS P4VP (PDP) matris ile, çift süreklilikteki çift gyroid morfolojisinde elde sistemi öz-montaj (Şekil 1b). PDP molekülleri seçici PS ağı (üzerine etanol ve P4VP zincirleri çöküşü çözülmüş olurŞekil 1c). Daha sonra, elektriksiz kaplama yöntemi kullanılarak, nikel şablon (Şekil 1d) gözenekleri içine yatırılır. Piroliz yoluyla geri kalan polimerin çıkarılmasından sonra, iyi düzenlenmiş bir gyroid nikel nanofoam (Şekil 1e) elde edilir.

<table border="1">
 <tbody>
 <tr>
 <td>REAGENTS:</td>
 <td></td>
 <td></td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP, CAS: 26222-40-2</td>
 <td>Polymer Source Inc.</td>
 <td>P9009-S4VP 
 P136-S4VP 
 P5462-S4VP 
 P3912-S4VP</td>
 <td>additional information are provided in a separate table</td>
 </tr>
 <tr>
 <td>PDP</td>
 <td>Aldrich</td>
 <td>P4402-100G-A</td>
 <td>recrystallized twice from petroleum ether</td>
 </tr>
 <tr>
 <td>SnCl2</td>
 <td>Acros Organics</td>
 <td>196981000</td>
 <td></td>
 </tr>
 <tr>
 <td>PdCl2</td>
 <td>Aldrich</td>
 <td>76050</td>
 <td></td>
 </tr>
 <tr>
 <td>NiSO4 x H2O</td>
 <td>Sigma-Aldrich</td>
 <td>227676</td>
 <td></td>
 </tr>
 <tr>
 <td>lactic acid</td>
 <td>Aldrich</td>
 <td>W261106</td>
 <td></td>
 </tr>
 <tr>
 <td>citric acid trisodium salt</td>
 <td>Sigma-Aldrich</td>
 <td>C3674</td>
 <td></td>
 </tr>
 <tr>
 <td>borane dimethyl amine complex</td>
 <td>Aldrich</td>
 <td>180238</td>
 <td></td>
 </tr>
 <tr>
 <td>PS-b-P4VP catalogue number</td>
 <td>Mn (PS), g/mol</td>
 <td>Mn(P4VP), g/mol</td>
 <td>PDI</td>
 </tr>
 <tr>
 <td>P9009-S4VP</td>
 <td>24000</td>
 <td>9500</td>
 <td>1.1</td>
 </tr>
 <tr>
 <td>P136-S4VP</td>
 <td>31900</td>
 <td>13200</td>
 <td>1.08</td>
 </tr>
 <tr>
 <td>P5462-S4VP</td>
 <td>37500</td>
 <td>16000</td>
 <td>1.3</td>
 </tr>
 <tr>
 <td>P3912-S4VP</td>
 <td>41500</td>
 <td>17500</td>
 <td>1.07</td>
 </tr>
 </tbody>
</table>

gyroid nickel nanostructures from diblock copolymer supramolecules

Nanoporous metal köpükler, benzersiz bir özellikler kombinasyonuna sahip olan - bunlar, termal ve elektriksel olarak iletken, katalitik olarak aktif olan ve bundan başka, yüksek gözeneklilik ve yüksek bir yüzey-hacim-ve ağırlık-ağırlık oranına sahiptir. Ne yazık ki, metalik Nano hazırlanması için genel yaklaşımlar, mekanik özellikleri üzerinde olumsuz bir etkiye sahip olabilir son derece bozuk mimari malzeme ile işlenir. Blok kopolimerleri sipariş Nano halinde kendi kendine birleşebilen yeteneğine sahip ve iyi sıralı metal nanofoams hazırlanması için şablon olarak uygulanabilir. Burada bir blok kopolimer-esaslı supramoleküler kompleksinin uygulamasını tarif - polistiren-blok-poli (4-vinilpiridin) (pentadesilfenol) PS-b-P4VP (PDP) - iyi sıralı nikel nanofoam için bir ön-madde olarak. Supramoleküler kompleksleri geleneksel blok kopolimerleri benzer bir faz davranışı sergiler ve iki-sürekli olmakta gyroid morfolojisi wit halinde kendi kendine birleşebilen olabilirBir P4VP (PDP) matris içinde yerleştirilmiş iki saat PS ağlar. PDP metal ile geri dolduruldu edilebilir gözenekli bir yapının oluşumuna yol açan, etanol içinde çözündürülebilir. Elektriksiz kaplama tekniği kullanılarak, nikel şablonunun kanal içine sokulabilir. Son olarak, kalan polimer ters gyroid morfolojisi olan nano gözenekli nikel bir köpük olarak elde edilen polimer / inorganik nanohibrit ikinci piroliz yolu ile uzaklaştırılabilir.

. Supramoleküler komplekslerinin morfolojisi PS-b-P4VP (PDP) x TEM ve SAXS Şekil 2a tarafından incelenir ve bir temsilcisi supramoleküler kompleksinin tipik gyroid modellerini görüntülemek 2b: çift dalga ve temsil bilinmektedir vagon teker desenleri (211) üzerinden ve çıkıntılar sırasıyla gyroid birim hücre (111) düzlemi,. P4VP (PDP) x blok etki nedeniyle iyot boyama koyu görünür iken PS blok etki parlak görünür. Şekil 2c dönemsellik it...

Watch this Scientific Journal Video about Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules at JoVE.com

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Bu makalede, kendi kendine bir araya iki bloklu kopolimer esaslı supramolecules elde edilen nano gözenekli şablon üzerine akımsız metal kaplama ile de sıralı nikel nanofoams hazırlanmasını tarif etmektedir.

Buradaki iki bloklu kopolimer Supramolecules ikinci Gyroid Nikel Nanoyapılar

Nanoporous metal foams possess a unique combination of properties - they are catalytically active, thermally and electrically conductive, and furthermore, ...

gyroid-nickel-nanostructures-from-diblock-copolymer-supramolecules

Research

JoVE Journal

Chemistry

12.3K Görüntüleme.  University of Groningen.  Bu makalede, kendi kendine bir araya iki bloklu kopolimer esaslı supramolecules elde edilen nano gözenekli şablon üzerine akımsız metal kaplama ile de sıralı nikel nanofoams hazırlanmasını tarif etmektedir. 

Video: Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Nucleoside Triphosphates - From Synthesis to Biochemical Characterization

The traditional strategy for the introduction of chemical functionalities is the use of solid-phase synthesis by appending suitably modified phosphoramidite precursors to the nascent chain. However, the conditions used during the synthesis and the restriction to rather short sequences hamper the applicability of this methodology. On the other hand, modified nucleoside triphosphates are activated building blocks that have been employed for the mild introduction of numerous functional groups into nucleic acids, a strategy that paves the way for the use of modified nucleic acids in a wide-ranging palette of practical applications such as functional tagging and generation of ribozymes and DNAzymes. One of the major challenges resides in the intricacy of the methodology leading to the isolation and characterization of these nucleoside analogues.
	
	In this video article, we present a detailed protocol for the synthesis of these modified analogues using phosphorous(III)-based reagents. In addition, the procedure for their biochemical characterization is divulged, with a special emphasis on primer extension reactions and TdT tailing polymerization. This detailed protocol will be of use for the crafting of modified dNTPs and their further use in chemical biology.

The protocol described herein aims to explain and abridge the numerous obstacles in the way of the intricate route leading to modified nucleoside triphosphates. Consequently, this protocol facilitates both the synthesis of these activated building-blocks and their availability for practical applications.

Nükleosid trifosfatlar - sentezinden Biyokimyasal Karakterizasyonu için

The  traditional strategy for the introduction of chemical functionalities is the  use of solid-phase synthesis by appending suitably modified ...

Kimya

Synthesis of Ligand-free CdS Nanoparticles within a Sulfur Copolymer Matrix

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature solvents. These coordinating ligands help solubilize and stabilize the nanoparticles while in solution, and can influence the resulting size and reactivity of the nanoparticles during their formation. Despite the ubiquity of using ligands during synthesis, the presence of aliphatic ligands on the nanoparticle surface can result in a number of problems during the end use of the nanoparticles, necessitating further ligand stripping or ligand exchange procedures. We have developed a way to synthesize cadmium sulfide (CdS) nanoparticles using a unique sulfur copolymer. This sulfur copolymer is primarily composed of elemental sulfur, which is a cheap and abundant material. The sulfur copolymer has the advantages of operating both as a high temperature solvent and as a sulfur source, which can react with a cadmium precursor during nanoparticle synthesis, resulting in the generation of ligand free CdS. During the reaction, only some of the copolymer is consumed to produce CdS, while the rest remains in the polymeric state, thereby producing a nanocomposite material. Once the reaction is finished, the copolymer stabilizes the nanoparticles within a solid polymeric matrix. The copolymer can then be removed before the nanoparticles are used, which produces nanoparticles that do not have organic coordinating ligands. This nascent synthesis technique presents a method to produce metal-sulfide nanoparticles for a wide variety of applications where the presence of organic ligands is not desired.

Herein we present a method to synthesize ligand-free cadmium sulfide (CdS) nanoparticles based on a unique sulfur copolymer. The sulfur copolymer operates as a high temperature solvent and a sulfur source during the nanoparticle synthesis and stabilizes the nanoparticles after the reaction.

Bir Kükürt Kopolimer Matrix içinde ligand-serbest CdS Nanopartiküller Sentezi

Aliphatic ligands are typically used during the synthesis of nanoparticles to help mediate their growth in addition to operating as high-temperature ...

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &#960;-&#960; Stacking Interactions

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE). Characterization of the copolymer revealed a narrow molecular distribution (PDI &#60; 1.03) and confirmed the degree of polymerization of mPEG122-b-(PheGE)15. The critical micelle concentration of the copolymer was evaluated using an established fluorescence method with the aggregation behavior evaluated by dynamic light scattering and transmission electronic microscopy. The potential of the copolymer for use in drug delivery applications was evaluated in a preliminary manner including in vitro biocompatibility, loading and release of the hydrophobic anti-cancer drug doxorubicin (DOX). A stable micelle formulation of DOX was prepared with drug loading levels up to 14% (wt%), drug loading efficiencies &#62; 60% (w/w) and sustained release of drug over 4 days under physiologically relevant conditions (acidic and neutral pH, presence of albumin). The high drug loading level and sustained release is attributed to stabilizing &#960;-&#960; interactions between DOX and the core-forming block of the micelles.

Anionic Polymerization of an Amphiphilic Copolymer for Preparation of Block Copolymer Micelles Stabilized by &amp;#960;-&amp;#960; Stacking Interactions

The key steps of living anionic polymerization of phenyl glycidyl ether (PheGE) on methoxy-polyethylene glycol (mPEG-b-PPheGE) are described. The resulting block copolymer micelles (BCMs) were loaded with doxorubicin 14% (wt%) and sustained release of drug over 4 days under physiologically relevant conditions was obtained.

π-π İstifleme etkileşimlerle Stabilize blok kopolimer miselleri hazırlanması için bir amfifilik kopolimerin anyonik polimerizasyonu

In this study, an amphiphilic copolymer that includes a core-forming block with phenyl groups was synthesized by living anionic polymerization of phenyl ...

Facet-to-facet Linking of Shape-anisotropic Colloidal Cadmium Chalcogenide Nanostructures

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be covalently and site-specifically linked via their end facets, resulting in polymer-like linear or branched chains. The linking procedure begins with a cation-exchange process in which the end facets of the cadmium chalcogenide NCs are first converted to silver chalcogenide. This is followed by the selective removal of ligands at their surface. This results in cadmium chalcogenide NCs with highly reactive silver chalcogenide end facets that spontaneously fuse upon contact with each other, thereby establishing an interparticle facet-to-facet attachment. Through the judicious choice of precursor concentrations, an extensive network of linked NCs can be produced. Structural characterization of the linked NCs is carried out via low- and high-resolution transmission electron microscopy (TEM), as well as energy-dispersive X-ray spectroscopy, which confirm the presence of silver chalcogenide domains between chains of cadmium chalcogenide NCs.

A protocol detailing how shape-anisotropic colloidal cadmium chalcogenide nanocrystals can be covalently linked via their end facets is presented here.

Model model şekil-Yönbağımlı kolloidal kadmiyum Chalcogenide taşınımı bağlama

Here, we describe a protocol that allows for shape-anisotropic cadmium chalcogenide nanocrystals (NCs), such as nanorods (NRs) and tetrapods (TPs), to be ...

Synthesis of Platinum-nickel Nanowires and Optimization for Oxygen Reduction Performance

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen reduction reaction. Spontaneous galvanic displacement was used to deposit Pt layers onto Ni nanowire substrates. The synthesis approach produced catalysts with high specific activities and high Pt surface areas. Hydrogen annealing improved Pt and Ni mixing and specific activity. Acid leaching was used to preferentially remove Ni near the nanowire surface, and oxygen annealing was used to stabilize near-surface Ni, improving durability and minimizing Ni dissolution. These protocols detail the optimization of each post-synthesis processing step, including hydrogen annealing to 250 &#176;C, exposure to 0.1 M nitric acid, and oxygen annealing to 175 &#176;C. Through these steps, Pt-Ni nanowires produced increased activities more than an order of magnitude than Pt nanoparticles, while offering significant durability improvements. The presented protocols are based on Pt-Ni systems in the development of fuel cell catalysts. These techniques have also been used for a variety of metal combinations, and can be applied to develop catalysts for a number of electrochemical processes.

&#160; The protocol describes the synthesis and electrochemical testing of platinum-nickel nanowires. Nanowires were synthesized by the galvanic displacement of a nickel nanowire template. Post-synthesis processing, including hydrogen annealing, acid leaching, and oxygen annealing were used to optimize nanowire performance and durability in the oxygen reduction reaction.

Platin-nikel Nanowires ve oksijen azaltma performansı için en iyi duruma getirme sentezi

Platinum-nickel (Pt-Ni) nanowires were developed as fuel cell electrocatalysts, and were optimized for the performance and durability in the oxygen ...

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of NixNb1-xO nanoparticles with different atomic compositions (x = 0.03, 0.08, 0.15, and 0.20) have been prepared by chemical precipitation. These NixNb1-xO catalysts are characterized by X-ray diffraction, X-ray photoelectron spectroscopy, and scanning electron microscopy. The study revealed the sponge-like and fold-like appearance of Ni0.97Nb0.03O and Ni0.92Nb0.08O on the NiO surface, and the larger surface area of these NixNb1-xO catalysts, compared with the bulk NiO. Maximum surface area of 173 m2/g can be obtained for Ni0.92Nb0.08O catalysts. In addition, the catalytic hydroconversion of lignin-derived compounds using the synthesized Ni0.92Nb0.08O catalysts have been investigated.

Chemical Precipitation Method for the Synthesis of Nb2O5 Modified Bulk Nickel Catalysts with High Specific Surface Area

A protocol for the synthesis of sponge-like and fold-like Ni1-xNbxO nanoparticles by chemical precipitation is presented.

Nb2O5 sentezi için kimyasal yağış yöntemi toplu nikel katalizör yüksek belirli yüzey alanı ile modifiye

We demonstrate a method for the synthesis of NixNb1-xO catalysts with sponge-like and fold-like nanostructures. By varying the Nb:Ni ratio, a series of ...

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We present methods for depositing and passively manipulating C60 molecules on rippled graphene that advance the pursuit of realizing applications involving 1D C60/graphene hybrid structures. The techniques applied in this exposition are geared towards high vacuum systems with preparation areas capable of supporting molecular deposition as well as thermal annealing of the samples. We focus on C60 deposition at low pressure using a homemade Knudsen cell connected to a scanning tunneling microscopy (STM) system. The number of molecules deposited is regulated by controlling the temperature of the Knudsen cell and the deposition time. One-dimensional (1D) C60 chain structures with widths of two to three molecules can be prepared via tuning of the experimental conditions. The surface mobility of the C60 molecules increases with annealing temperature allowing them to move within the periodic potential of the rippled graphene. Using this mechanism, it is possible to control the transition of 1D C60 chain structures to a hexagonal close packed quasi-1D stripe structure.

Preparation and Characterization of C60/Graphene Hybrid Nanostructures

Here we present a protocol for the fabrication of C60/graphene hybrid nanostructures by physical thermal evaporation. Particularly, the proper manipulation of deposition and annealing conditions allow the control over the creation of 1D and quasi 1D C60 structures on rippled graphene.

C60/Graphene hibrid nanoyapıların malzemelerin hazırlık ve

Physical thermal deposition in a high vacuum environment is a clean and controllable method for fabricating novel molecular nanostructures on graphene. We ...

Disentangling High Strength Copolymer Aramid Fibers to Enable the Determination of Their Mechanical Properties

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to diversify the fiber choices in the United States body armor market, copolymer fibers based on the combination of 5-amino-2-(p-aminophenyl) benzimidazole (PBIA) and the more conventional PPTA were introduced. Little is known regarding the long-term stability of these fibers, but as condensation polymers, they are expected to have potential sensitivity to moisture and humidity. Therefore, characterizing the strength of the materials and understanding their vulnerability to environmental conditions is important for evaluating their use lifetime in safety applications. Ballistic resistance and other critical structural properties of these fibers are predicated on their strength. To accurately determine the strength of the individual fibers, it is necessary to disentangle them from the yarn without introducing any damage. Three aramid-based copolymer fibers were selected for the study. The fibers were washed with acetone followed by methanol to remove an organic coating that held the individual fibers in each yarn bundle together. This coating makes it difficult to separate single fibers from the yarn bundle for mechanical testing without damaging the fibers and affecting their strength. After washing, fourier transform infrared (FTIR) spectroscopy was performed on both washed and unwashed samples and the results were compared. This experiment has shown that there are no significant variations in the spectra of poly(p-phenylene-benzimidazole-terephthalamide-co-p-phenylene terephthalamide) (PBIA-co-PPTA1) and PBIA-co-PPTA3 after washing, and only a small variation in intensity for PBIA. This indicates that the acetone and methanol rinses are not adversely affecting the fibers and causing chemical degradation. Additionally, single fiber tensile testing was performed on the washed fibers to characterize their initial tensile strength and strain to failure, and compare those to other reported values. Iterative procedural development was necessary to find a successful method for performing tensile testing on these fibers.

The primary goal of the study is to develop a protocol to prepare consistent specimens for accurate mechanical testing of high strength copolymer aramid fibers, by removing a coating and disentangling the individual fiber strands without introducing significant chemical or physical degradation.

Disentangling yüksek mukavemetli kopolimer Aramid Elyaf mekanik özelliklerinin belirlenmesi etkinleştirmek için

Traditionally, soft body armor has been made from poly(p-phenylene terephthalamide) (PPTA) and ultra-high molecular weight polyethylene. However, to ...

Stable DNA Motifs, 1D and 2D Nanostructures Constructed from Small Circular DNA Molecules

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D DNA nanostructures. Over decades, the rapid development of DNA nanotechnology is attributed to the use of linear DNAs as the source materials. For example, the DAO (double crossover, antiparallel, odd half-turns) tile is well-known as a building block for construction of 2D DNA lattices; the core structure of DAO is made from two linear single-stranded (ss) oligonucleotides, like two ropes making a right hand granny&#160;knot. Herein, a new type of DNA tiles called cDAO (coupled DAO) are built using a small circular ss-DNA of c64nt or c84nt (circular 64 or 84 nucleotides) as the scaffold strand and several linear ss-DNAs as the staple strands. Perfect 1D and 2D nanostructures are assembled from cDAO tiles: infinite nanowires, nanospirals, nanotubes, nanoribbons; and finite nano-rectangles. Detailed protocols are described: 1) preparation by T4 ligase and purification by denaturing PAGE (polyacrylamide gel electrophoresis) of small circular oligonucleotides, 2) annealing of stable circular tiles, followed by native PAGE analysis, 3) assembling of infinite 1D nanowires, nanorings, nanospirals, infinite 2D lattices of nanotubes and nanoribbons, and finite 2D nano-rectangles, followed by AFM (Atomic Force Microscopy) imaging. The method is simple, robust, and affordable for most labs.

This article presents a detailed protocol for T4 ligation and denaturing PAGE purification of small circular DNA molecules, annealing and native PAGE analysis of circular tiles, assembling and AFM imaging of 1D and 2D DNA nanostructures, as well as agarose gel electrophoresis and centrifugation purification of finite DNA nanostructures.

İstikrarlı DNA motifleri, 1D ve 2D nanoyapıların küçük dairesel DNA molekülleri inşa

This article presents a detailed protocol for synthesis of small circular DNA molecules, annealing of circular DNA motifs, and construction of 1D and 2D ...

Gene-therapy Inspired Polycation Coating for Protection of DNA Origami Nanostructures

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in physiological fluids induce denaturation and degradation of self-assembled DNA nanostructures. In non-viral gene delivery, enzymatic degradation of DNA is overcome by the encapsulation of the negatively charged DNA in a cationic shell. Herein, inspired by gene delivery advancements, a simple, one-step and robust methodology is presented for the stabilization of DNA origami nanostructures by coating them with chitosan and linear polyethyleneimine. The polycation coating efficiently protects DNA origami nanostructures in Mg-depleted and nuclease-rich media. This method also preserves the full addressability of enzyme- and aptamer-based functionalization of DNA nanostructures.

Here, a protocol for the protection of DNA origami nanostructures in Mg-depleted and nuclease-rich media using natural cationic polysaccharide chitosan and synthetic linear polyethyleneimine (LPEI) coatings is presented.

Gen terapisi Polycation kaplama DNA Origami nanoyapıların korunması için ilham.

DNA origami nanostructures hold an immense potential to be used for biological and medical applications. However, low-salt conditions and nucleases in ...