Wir danken für die finanzielle Unterstützung durch die Zernike-Institut für Neue Materialien, Universität Groningen.

1. Herstellung und Charakterisierung von PS-b-P4VP (PDP)-Komplexe mit Doppel Gyroid Morphologie <ol><li> Abwiegen Polystyrol-block-poly (4-Vinylpyridin) (PS-b-P4VP) und Pentadecylphenol (PDP, M r = 304,51 g / mol). Um die Gyroid Morphologie zu erhalten, sorgfältig wählen Sie die Menge der PDP sollte (der Gewichtsanteil der P4VP (PDP) Block (f P4VP (PDP)) sollte ca.. 0,6 nach dem Phasendiagramm von linearen AB-Diblock-Copolymere). Normalerweise 0,15-0,2 g eines PS-b-P4VP zu PS-b-P4VP (PDP)-Filme 50-100 um dick (vorausgesetzt, dass der Durchmesser eines in dem Schritt 1.3 verwendet Petrischale ist 5-6 cm). Berechnen der Menge des PDP gemäß der folgenden Gleichungen: <img alt="Gleichung 1" src="/files/ftp_upload/50673/50673eq1.jpg" /> <img alt="Gleichung 2" src="/files/ftp_upload/50673/50673eq2.jpg" /> <img alt="Gleichung 3" src="/files/ftp_upload/50673/50673eq3.jpg" /><br/&gt; <img alt="Gleichung 4" src="/files/ftp_upload/50673/50673eq4.jpg" /></li><li> Lösen PS-b-P4VP und PDP in Chloroform und rühren Sie es für ein paar Stunden bei Raumtemperatur. Aufrechterhaltung der Konzentration des Polymers unter 2 Gew.%, um die homogene Komplexbildung sicherzustellen. </li><li> Füllen Sie die Lösung in eine Glaspetrischale. </li><li> Die Schale in eine gesättigte Chloroform-Atmosphäre. </li><li> Nach etwa einer Woche, nehmen Sie die Petrischale. Ein Film der supramolekularen Komplex. </li><li> Trocknen des Films im Vakuum bei 30 ° C über Nacht. </li><li> Legen Sie den Film in einem speziellen Behälter, entfernen Sie die Luft aus dem Behälter und füllen Sie ihn dann mit Stickstoff. Annealing der Film für 4 Tage im Ofen bei 120 ° C unter N 2-Atmosphäre mit 1 bar Überdruck. </li><li> Schneiden Sie das kleine Stück des Films, in Epoxidharz eingebettet werden und Heilung über Nacht bei 40 ° C </li><li> Mikrotom der Probe auf eine Dicke von etwa 80 nm unter Verwendung eines Diamantmessers bei Raumtemperatur. ThE Mikrotom Abschnitt wird auf dem Wasser schwimmen. Holen sie und legen auf Cu Netze. </li><li> Setzen Sie die Gitter, die die Abschnitte Mikrotom in einem Glas mit Jod. Nach 45 min Proben sind gebeizt und bereit für die Transmissionselektronenmikroskopie. </li><li> Legen Sie die Cu-Gitter mit gefärbten Schnitten im Transmissions-Elektronenmikroskop bei einer Beschleunigungsspannung von 120 kV und Bild der Probe. </li><li> Legen Sie das Stück des Films (nach Schritt 1.7) erhalten in den Probenhalter für Kleinwinkel-Röntgenstreuung und fixieren Sie es mit einem Kapton-Band. Setzen Sie den Probenhalter vorbereitet in die Maschine für SAXS. Öffnen Sie die Röntgen-Shutter und erwerben die 2D-Streumuster. Integrieren Sie die erhaltenen 2D-Muster und die Position der Peaks in 1D-Muster zu analysieren. </li></ol> 2. Erzeugung und Charakterisierung der porösen Struktur <ol><li> Setzen Sie das Stück des Films (nach Schritt 1.7 erhalten) in Ethanol und halten Sie sie für drei Tage. </li><li> Trocknen Sie die Probe. </li><li> Prepare die Proben für 1 H-NMR-Messungen. PDP-Pulver aufzulösen, PS-b-P4VP Pulver supramolekularen Komplex PS-b-P4VP (PDP) (nach Schritt 1.7), und die poröse Schicht (nach Schritt 2.2) in CDCl 3. Record 1 H-NMR-Spektren bei Raumtemperatur. </li><li> Analyse PS-b-P4VP Pulver supramolekularen Komplex PS-b-P4VP (PDP) (nach Schritt 1.7), und poröse Folie (nach Schritt 2.2) durch Differential-Scanning-Kalorimetrie. Verwenden ein moduliertes mit einer Heiz / Kühlrate von 1 ° C / min, einer Schwingungsamplitude von 0,5 ° C und einer Schwingungsperiode von 60 Sekunden. Ins Gleichgewicht der Proben bei -30 ° C, Wärme bis 180 ° C, kühl bis -30 ° C, und dann wieder erhitzen auf 180 ° C Die Daten aus dem zweiten Erwärmungszyklus für die Analyse. </li><li> Ausgasen die poröse Probe (nach Schritt 2.2) für 8 h bei Raumtemperatur und 18 h bei 70 ° C durchzuführen und die Stickstoffadsorption bei 77 K. </li><li> Verwenden Sie die entsprechende Software (zB WinADP) und Modelle, um die erhaltenen Isothermen analysieren. </li><li> Trocknen der porösen Probe (nach Schritt 2.2) bei 50 ° C für 8 h und Entgasen bei Raumtemperatur und einem Druck von 0,5 Pa während 2 Stunden. </li><li> Führen Quecksilberporosimetrie. </li></ol> 3. Einfügen Nickel in der Polymer-Vorlage <ol><li> Wiegen Sie Zinnchlorid (SnCl 2, M r = 189.60 g / mol) und bereiten eine wässrige Lösung (0,1 M SnCl 2 / 0,1 M HCl, 1.896 g 100 ml H 2 O SnCl 2, 0,8 ml HCl, und). Setzen Sie die Lösung auf einem Schüttler über Nacht, um die vollständige Auflösung von SnCl 2 zu gewährleisten. </li><li> Wiegen Sie Palladiumchlorid (PdCl 2, M r = 177.33 g / mol) und bereiten eine wässrige Lösung (0,0014 M PdCl 2 / 0,25 M HCl, 0,025 g 100 ml H 2 O PdCl 2, 2 ml HCl und). </li><li> Bereiten Sie Teil 1 des Nickelgalvanisierbad: wiegen 6,78 g Nickelsulfat-Hexahydrat (NiSO 4 • 6 H 2 O, M r = 262, 85 g / mol) und 2 g Natriumcitrat (Na 3 C 6 H 5 O 7, M r = 258.06 g / mol) und 80 ml ​​Wasser auflösen. Add 828 ul 85% ige Milchsäure (C 3 H 6 O 3, M r = 90,08 g / mol). </li><li> Bereiten Sie Teil 2 der Nickelgalvanisierbad: Gewicht aus 0,2 g Borandimethylaminkomplexes ((CH 3) 2 NHBH 3, M r = 58,92 g / mol) und löst ihn in 20 ml Wasser. Borandimethylaminkomplexes sollte in einem gut gelüfteten Abzug gehandhabt werden. </li><li> Tauchen der porösen Folie (nach Schritt 2.2) in der wässrigen Lösung von Zinnchlorid (Schritt 3.1) für 1 Stunde. </li><li> Spülen Sie den Film gründlich mit VE-Wasser. </li><li> Tauchen der Folie in der wässrigen Lösung von Palladiumchlorid (Stufe 3.2) für 1 Stunde. </li><li> Spülen Sie den Film gründlich mit VE-Wasser. </li><li> Mix Teil 1 (3.3) und Teil 2 (3.4) des Nickelgalvanisierbad. Einstellen des pH auf 7,0 mit Ammoniumhydroxid. </li><li> Tauchen der Folie in der Nickel-Plattierungsbad für 1 Stunde. </li><li> Spülen Sie den Film gründlich mit VE-Wasser. </li><li> Trocknen Sie die Probe. </li><li> Bereiten Sie die Probe überzogen für die Elektronenmikroskopie wie in Schritten von 1,8 bis 1,9 beschrieben. </li><li> Bild der Probe, wie in Schritt 1.11 beschrieben. </li><li> Legen Cu Gitter enthält die Abschnitte des beschichteten Probe in der hochauflösenden Transmissionselektronenmikroskop. Erwerben Sie hochauflösende TEM-Aufnahmen. Beachten Sie die Probe unter dem Mikroskop, und wählen Sie den Bereich für die Elementanalyse mittels EDX (Energie-Streuungsanalyse von X-Rays). Führen Sie die EDX-Analyse des gewählten Bereich und analysieren die erhaltenen Muster. </li></ol> 4. Exposition der Inverse Gyroid Nickel Schaum <ol><li> Setzen Sie den vernickelt Film (nach Schritt 3.12) in einem Ofen bei 350 ° C und halten Sie sie von 1 Stunde bis zu 4 Tage. </li><li> Bringen Sie die Probe in die Probenhalter mit einem Silberpaste. </li><li> Legen Sie die Probe in die Raster-Elektronen-micROSCOPE. Erwerben mehrerer Bilder der Probe. </li><li> Legen Sie die Probe in die Raster-Elektronen-Mikroskop. Beachten Sie die Probe unter dem Mikroskop, und wählen Sie den Bereich für die Elementanalyse mittels EDX. Führen Sie die EDX-Analyse des gewählten Bereich und analysieren die erhaltenen Muster. </li></ol>

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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>

Die Autoren erklären, keine finanziellen Interessen konkurrieren.

Supramolekulare Komplexe erfolgreich als Vorstufen für geordneten Metall-Nanoschäumen aufgebracht. Bei diesem Verfahren ist der entscheidende Schritt, um die entsprechende Vorlage erfassen, dh eine Vorlage mit Gyroid Morphologie. In dem Phasendiagramm von Blockcopolymeren der Gyroid Bereich ist sehr klein und es ist ziemlich schwierig, vorbei. Dies bedeutet, dass, wenn herkömmliche Blockcopolymere werden als Ausgangsmaterialien verwendet werden, hat die recht aufwendige Synthese, bis die gewünschte Zusammen...

Es gibt verschiedene Techniken zur Herstellung von Metall-Nanoschäumen zur Verfügung: Legierungsauflösung 1-3, Sol-Gel 4,5 nähert, nanosmelting 6,7, und die Verbrennungssynthese 8. Im Entlegierung Verfahren ist das Ausgangsmaterial in der Regel eine binäre Legierung, beispielsweise eine Legierung aus Silber und Gold. Das weniger edle Metall, Silber in diesem Fall kann entweder chemisch oder elektrochemisch, was zu einer ungeordneten porösen Schaum mit Goldnanogröße Bänder entfernt werden. In Verbrennungssynthese, Metall gemischt mit einer energetischen Vorläufer, die Energie während der Zersetzung Mitteilungen und treibt die Bildung von Metall-Nanoschaum 8. Studien über das mechanische Verhalten von Metallschäumen zeigen, dass in ungeordneten Architekturen Spannungen nicht effektiv aus dem Ligamentum nanoskaligen zur Gesamtmakro 9-11 übertragen werden. Somit wird erwartet geordneten Metallnanoschäume, überlegene mechanische Eigenschaften im Vergleich zu der habenungeordneten diejenigen. Die Idee hier dargestellt wird, ist von Blockcopolymeren, die Selbstorganisation in geordnete Nanostrukturen als Vorläufer von Metall-Nanoschäumen zu beschäftigen. Je nach der Zusammensetzung eines Block-Copolymers, wobei die Gesamtzahl der Monomer-Einheiten und dem Ausmaß der Abstoßung zwischen den chemisch verbundenen Blöcken, werden verschiedene Morphologien wie: sphärisch, zylindrisch, lamellare Doppel Gyroid hexagonal perforierte lamellare und andere 12-14 . Weiterhin können Polymerblöcke selektiv die zu nanoporösen Materialien 15 abgebaut werden kann. Die häufigsten Methoden sind: Ozonolyse 16-18, UV-Bestrahlung 19, Reactive Ion Etching 20-22, 23-26 und Auflösung. Die erzeugten porösen Strukturen können mit verschiedenen anorganischen Materialien verfüllt werden. Metalloxide (z. B. SiO 2, TiO 2) werden üblicherweise durch ein Sol-Gel-Verfahren in der Vorlage Kanäle 27-29 eingeführt. Electrochemical und stromloses Plattieren werden häufig verwendet, um Metall in oder auf Vorlagen 30-33 abzuscheiden. Schließlich kann das restliche Polymer aus dem Polymer / anorganische Nanohybrid 2 durch Pyrolyse, Auflösung 34,35, 28,29 UV-Abbau, usw. entfernt werden In unserem Ansatz gehen wir von einem supramolekularen Komplex von Polystyrol-block-poly (4-Vinylpyridin) (PS-b-P4VP) Diblock-Copolymer und amphiphilen Pentadecylphenol (PDP)-Molekülen. Dieser Komplex ist ein Ergebnis der Wasserstoffbrückenbindung zwischen PDP und Pyridinringe (Abbildung 1a). Die Zusammensetzung des Startblock-Copolymer und die Menge an zugesetztem PDP sind derart gewählt, dass die erhaltene System Selbstorganisation in der bikontinuierlichen Doppel Gyroid Morphologie mit einem PS-Netz und einem P4VP (PDP)-Matrix (Abbildung 1b). PDP-Moleküle selektiv in Ethanol und P4VP Ketten Zusammenbruch aufgelöst auf die PS-Netzwerk (Abbildung 1c). Anschließend wurde unter Verwendung stromloses Verfahren, Nickel in die Poren der Schablone (1d) aufgebracht. Nach dem Entfernen des verbleibenden Polymers durch Pyrolyse wird eine geordnete Gyroid Nickel-Nanoschaum, erhalten (Fig. 1e).

<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

Nanoporöse Metallschäume besitzen eine einzigartige Kombination von Eigenschaften - sie sind katalytisch aktive, thermisch und elektrisch leitfähig ist, und außerdem eine hohe Porosität, hohe Oberflächen-zu-Volumen und Kraft-zu-Gewicht-Verhältnis. Leider gemeinsame Ansätze zur Herstellung von metallischen Nanostrukturen machen Materialien mit stark fehl Architektur, die sich nachteilig auf ihre mechanischen Eigenschaften haben könnten. Block-Copolymere haben die Fähigkeit zur Selbstorganisation in geordnete Nanostrukturen und können als Vorlage für die Herstellung von geordneten Metall-Nanoschäumen verwendet werden. Hier beschreiben wir die Verwendung eines Blockcopolymers supramolekularen Komplex - Polystyrol-block-poly (4-vinylpyridin) (Pentadecylphenol) PS-b-P4VP (PDP) - als Vorstufe für geordneten Nickel-Nanoschaum. Die supramolekulare Komplexe weisen eine Phasenverhalten ähnlich wie bei herkömmlichen Blockcopolymeren und Selbstorganisation in den bikontinuierlich Gyroid Morphologie Witzh zwei PS-Netzwerke in einem P4VP (PDP)-Matrix angeordnet. PDP kann in Ethanol, die zur Bildung einer porösen Struktur, die mit Metall aufgefüllt werden kann, gelöst werden. Mit stromloses Technik kann Nickel in der Vorlage Kanäle eingesetzt werden. Schließlich kann das verbleibende Polymer durch Pyrolyse aus der Polymer / anorganische Nanohybrid wodurch nanoporösen Nickelschaum mit inverser Gyroid Morphologie entfernt werden.

. Die Morphologie der supramolekularen Komplexen PS-b-P4VP (PDP) x durch TEM und SAXS untersucht den 2a und 2b typischen Gyroid Muster einer repräsentativen supramolekularen Komplex an: das Doppel-Welle und die Wagen-Rad-Muster, die bekannt ist, darstellen, werden Vorsprünge durch die (211) und die (111)-Ebene des Gyroid Einheitszelle sind. Die PS-Block Domains hell erscheinen, während die P4VP (PDP) x Block Domains dunkel erscheinen aufgrund Iodfärbung. 2c...

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

Gyroid Nickel Nanostructures from Diblock Copolymer Supramolecules

Dieser Artikel beschreibt die Herstellung von geordneten Nickel-Nanoschäumen über stromlose Metallabscheidung auf nanoporösen Vorlagen aus selbstorganisierten Diblock-Copolymer auf Basis Supramoleküle erhalten.

Gyroid Nickel Nanostrukturen aus Diblockcopolymer Übermolekülen

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 Aufrufe.  University of Groningen.  Dieser Artikel beschreibt die Herstellung von geordneten Nickel-Nanoschäumen über stromlose Metallabscheidung auf nanoporösen Vorlagen aus selbstorganisierten Diblock-Copolymer auf Basis Supramoleküle erhalten. 

Serie: 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.

Nucleosidtriphosphaten - von der Synthese zur biochemischen Charakterisierung

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

Forschung

Chemie

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.

Synthese von Ligand freien CdS-Nanopartikel innerhalb eines Schwefel-Copolymer-Matrix

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.

Die anionische Polymerisation eines amphiphilen Copolymer zur Herstellung von Blockcopolymermicellen Stabilisiert durch π-π-Stapelwechselwirkungen

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.

Facette für Facette Verknüpfung von Form-anisotropen kolloidales Cadmium Chalkogenid Nanostrukturen

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.

Synthese von Platin-Nickel Nanodrähte und Optimierung für Sauerstoff Leistung

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.

Chemischen Niederschlag-Methode für die Synthese von Nb2O5 geändert, Bulk-Nickel-Katalysatoren mit hoher spezifischer Oberfläche

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.

Herstellung und Charakterisierung von 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 ...

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.

Entwirren hohe Festigkeit-Copolymer-Aramid-Fasern um die Bestimmung der mechanischen Eigenschaften ermöglichen

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.

Stabile DNA-Motive, 1D und 2D Nanostrukturen aus kleinen kreisförmigen DNA-Moleküle gebaut

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.

Gentherapie inspiriert Polykation Beschichtung zum Schutz der DNA Origami Nanostrukturen

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