Name: synthesis and reaction chemistry of nanosize monosodium titanate
Uploaded: 2016-02-23T14:00:00.000+00:00
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Description: Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

The authors thank the Laboratory Directed Research and Development program at the Savannah River National Laboratory (SRNL) for funding. We thank Dr. Fernando Fondeur for collection and interpretation of the FT-IR spectra and Dr. John Seaman of the Savannah River Ecology Laboratory for the use of the DLS instrument for particle size measurements. We also thank the Dr. Daniel Chan of the University of Washington and the National Institute of Health (Grant #1R01DE021373-01), for funding experiments investigating the ion exchange reactions with Au(III). The Savannah River National Laboratory is operated by Savannah River Nuclear Solutions, LLC for the Department of Energy under contract DE-AC09-08SR22470.

1. Synthese von Nano-Mononatrium-Titanat (nMST) <ol><li> Herstellung von 10 ml der Lösung 1 durch Zugabe von 0,58 ml 25 Gewichts-% Natriummethylat-Lösung zu 7,62 ml Isopropanol gefolgt von 1,8 ml Titanisopropoxid. </li><li> Herstellung von 10 ml der Lösung # 2 von 0,24 ml ultrareinem Wasser zu 9,76 ml Isopropanol hinzugefügt wird. </li><li> Hinzufügen von 280 ml Isopropanol in einen 3-Hals-500 ml-Rundkolben, gefolgt von 0,44 ml von Triton X-100 (durchschnittliches MW: 625 g / mol). Rühren Sie die Lösung gut mit einem magnetischen Rührstab. </li><li> Bereiten Sie einen Dual-Channel-Spritzenpumpe zu liefern Lösungen # 1 und # 2 mit einer Rate von 0,333 ml / min. </li><li> Last Lösungen # 1 und # 2 in zwei getrennte 10-ml-Spritzen mit einer Länge von Schlauch ausgestattet, die Lieferung der Lösung aus der Spritzenpumpe unter die Lösung Niveau in der 500-ml-Rundkolben ermöglichen. </li><li> Unter Rühren hinzu alle Lösungen # 1 und # 2 (je 10 ml) zur Reaktions die Spritzenpumpe in Schritt 1.4 programmiert werden. </li> &lt;li&gt; Nachdem die Zugabe beendet ist, die Kappe des Kolbens und weiter für 24 Stunden bei Raumtemperatur rühren. </li><li> Die Kappe des Kolbens und erhitzt das Reaktionsgemisch auf ~ 82 ° C (Rückfluß Isopropanol) für 45-90 min, gefolgt von Spülen mit Stickstoff unter Erhitzen erhalten. Als Isopropanol verdunstet ist, fügen intermittierend Reinstwasser das verdampfte Isopropanol zu ersetzen. </li><li> Nachdem das meiste des Isopropanol verdampft ist und das Volumen von Wasser gegeben ist ungefähr 50 ml, entfernen die Hitze und abkühlen lassen der Reaktionsmischung. </li><li> Sammeln Sie das Produkt durch Filtrieren durch ein 0,1-um-Nylonfilterpapier und wäscht mehrmals mit Wasser, das Tensid und restliche Isopropanol zu entfernen. Nicht bis zur Trockenheit filtern. Nach dem Waschen beendet ist, übertragen die Aufschlämmung aus dem Filter in einen vorgewogenen Flaschen oder Fläschchen, und speichern als eine wässrige Aufschlämmung. </li><li> Bestimmen Sie die Ausbeute durch die Gewichtsprozent Feststoffe aus dem Schlamm zu bestimmen. Dies kann durch Messen des Gewichts eines aliquoten Teils durchgeführt werdender Schlamm vor und nach dem Trocknen. </li></ol> 2. Au (III) Ion Exchange <ol><li> Übertragen 6,50 g von 4,23 Gew% nMST Aufschlämmung auf eine 50-ml-Zentrifugenröhrchen. Diese Menge kann auf dem tatsächlichen Gewichtsprozent des nMST Aufschlämmung in Stufe 1.10 vorstehend hergestellten variieren, und in Schritt 1.11 bestimmt. </li><li> Abwiegen 0,0659 g HAuCl 4 · 3H 2 O in einen 1-Dram Glasfläschchen. Die Ziel Ti: Au Massenverhältnis 4: 1. </li><li> Man löst das HAuCl 4 · 3H 2 O in ~ 1 ml Wasser, dann Transfer zum Zentrifugenröhrchen die nMST enthält. Spülen Sie die Fläschchen mehrmals mit zusätzlichem Wasser zu allen von der 3H HAuCl 4 · gewährleisten 2 O auf die Zentrifugenröhrchen überführt wird, um die nMST enthält. </li><li> Verdünnen der Suspension mit zusätzlichem Wasser, soweit erforderlich, um das Gesamtvolumen auf 11 ml zu bringen. Ziel eine abschließende Au (III) Konzentration von etwa 15 mM. </li><li> Wickeln Sie das Zentrifugenröhrchen in Folie der Suspension im Dunkeln zu halten, ist eind dann für mindestens 4 Tage, um die Suspension auf einem Schüttler Rotisserie fallen. </li><li> Sammeln Sie das Produkt bei 3.000 × g durch Zentrifugation für 15 Minuten um die Feststoffe zu isolieren. Wasche die Feststoffe dreimal mit destilliertem Wasser durch Redispergieren in Wasser, und durch Reisolat bei 3.000 xg für 15 min zentrifugiert jede nicht ausgetauschten Au (III) zu entfernen. </li><li> Lagern Sie das Endprodukt entweder als wässrige Suspension in Wasser redispergiert oder als feuchte Feststoff durch Dekantieren des letzten Waschwasser und Verschließen des Rohrs ab. Lagern Sie das Produkt in der Dunkelheit. </li></ol> 3. Herstellung der Peroxotitanate <ol><li> Übertragen werden 5 g einer 9,8 Gew% igen Aufschlämmung von nMST zu einem kleinen Kolben. </li><li> Man wiegt 0,154 g 30 Gew% H 2 O 2 Lösung. Die Ziel H 2 O 2: Ti-Molverhältnis 0,25: 1. </li><li> Unter Rühren hinzufügen, die nMST Suspension auch die 0,154 g H 2 O 2 -Lösung tropfenweise. Auf H 2 O 2 -Zugabe, die Aussetzung der WHIte Feststoffe dreht sich sofort gelb. </li><li> Nachdem die Zugabe abgeschlossen ist Rühre das Reaktionsgemisch bei Umgebungstemperatur für 24 Std. </li><li> Sammeln des Produkts durch Filtrieren durch einen 0,1-um-Nylonfilter und wäscht mehrmals mit Wasser nicht umgesetztes H 2 O 2 zu entfernen. Nicht bis zur Trockenheit filtern. Nach dem Waschen beendet ist, übertragen die Aufschlämmung aus dem Filter in einen vorgewogenen Flaschen oder Fläschchen, und speichern als eine wässrige Aufschlämmung. </li></ol>

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The authors have nothing to disclose.

Das Vorhandensein von Fremdwasser, beispielsweise von unreinen Reagenzien, kann das Ergebnis der Reaktion verändern, was zu einer größeren oder polydisperse Teilchen. Daher sollte darauf Trockenreaktanten verwendet werden geachtet werden. Das Titanisopropoxid und Natriummethoxid sollten bei Nichtgebrauch in einem Exsikkator gelagert werden. Hochreines Isopropanol sollte auch für die Synthese eingesetzt werden. Die Temperatur wurde gefunden aus einem Gel eine Schlüsselrolle bei der Umwan...

Titandioxid und Alkalimetalltitanaten sind in einer Vielzahl von Anwendungen wie beispielsweise Pigmente in Farben und Hautpflegemitteln und als Photokatalysatoren bei der Energieumwandlung und Nutzung weit verbreitet. 1-3 Sodium Titanate haben sich als wirksam erwiesen Materialien eine Reihe von Kationen zu entfernen, über einen weiten Bereich von pH-Bedingungen durch Kationenaustausch-Reaktionen. 4-7 Neben den Anwendungen gerade beschrieben, in Mikrometergröße Natriumtitanate und Natrium peroxotitanates haben gezeigt, auch als therapeutische Metall-Delivery-Plattform dienen vor kurzem. In dieser Anwendung therapeutischen Metallionen wie Au (III), Au (I) und Pt (II) für die Natriumionen von Mononatrium Titanat (MST). In vitro-Tests mit dem Edelmetall-ausgetauschten Titanate ausgetauscht zeigen Unterdrückung das Wachstum von Krebs und Bakterienzellen durch einen unbekannten Mechanismus. 8,9 Historisch gesehen, Natriumtitanate haben seinen erzeugt sowohl Sol-Gel und hydrothermalen Syntheseverfahren unter Verwendung von in feine Pulver mit Partikelgrößen resultieren mehreren hundert Mikrometern von wenigen reichen. 4,5,10,11 In jüngerer Zeit wurden synthetische Verfahren berichtet, dass nanoskaligem Titandioxid hergestellt, Metall- dotierten Titanoxiden, und eine Vielzahl von anderen Metall Titanate. Beispiele schließen Natrium Titanoxid-Nanoröhren (NaTONT) oder Nanodrähte durch Umsetzung von Titandioxid in überschüssigem Natriumhydroxid bei erhöhter Temperatur und Druck, 12-14 Natriumtitanat Nanofasern durch Umsetzung von Peroxotitansäure mit überschüssigem Natriumhydroxid bei erhöhter Temperatur und Druck, 15 und Natrium und Cäsium-Titanat-Nanofasern durch Delamination von säure ausgetauscht mikrometergroßen Titanate. 16 Die Synthese von nanoskaligen Natriumtitanate und Natrium peroxotitanates ist von Interesse, Ionenaustausch-Kinetik zu verbessern, die in der Regel von Film Diffusion oder Intrapartikel DIFFU gesteuert werdension. Diese Mechanismen werden weitgehend durch die Teilchengrße des Ionenaustauscher gesteuert. Zusätzlich als ein therapeutisches Metall Abgabeplattform, würde die Teilchengröße des Titanat-Material erwartet werden, signifikant die Natur der Wechselwirkung zwischen dem Metall-ausgetauschten Titanat und dem Krebs und Bakterienzellen zu beeinflussen. Beispielsweise Bakterienzellen, die typischerweise in der Größenordnung von 0,5 liegen - 2 um, müsste wahrscheinlich verschiedene Interaktionen mit mikrometergroßen Teilchen gegenüber Teilchen in Nanogröße. Zusätzlich wurden nicht-phagozytische eukaryotischen Zellen nur gezeigt, um Partikel internalisieren mit einer Größe von weniger als 1 Mikron. 17 Somit ist die Synthese von nanoskaligen Natrium Titanate auch von Interesse Metallabgabedüse und zelluläre Aufnahme vom Titanat Abgabeplattform zu erleichtern. Reduzieren der Größe von Natrium und Titanate peroxotitanates wird auch die effektive Kapazität in Metallion Trennungen erhöhen und photochemischen Eigenschaften des Materials zu verbessern. 16,18 &lt;/ sup&gt; Dieses Papier beschreibt ein Protokoll zur Synthese von nanoskaligen Mononatrium Titanat (nMST) unter milden Sol-Gel-Bedingungen 19 Die Herstellung des entsprechenden Peroxid modifiziert nMST entwickelt. zusammen mit einer Ionenaustauschreaktion werden die nMST mit Au (III) zu laden ebenfalls beschrieben.

<table><tbody><tr><td>Titanium(IV) isopropoxide</td><td>Sigma Aldrich</td><td>377996</td><td>99.999% trace metals basis</td></tr><tr><td>Isopropyl alcholol, 99.9%</td><td>Sigma Aldrich</td><td>650447</td><td>HPLC grade (Chomasolv)</td></tr><tr><td>Sodium methoxide in methanol</td><td>Sigma Aldrich</td><td>156256</td><td>25 wt%</td></tr><tr><td>Triton X-100</td><td>Sigma Aldrich</td><td>T9284</td><td>BioXtra</td></tr><tr><td>hydrogen tetrachloroaurate(III) trihydrate</td><td>Sigma Aldrich</td><td>G4022</td><td>ACS reagent grade</td></tr><tr><td>hydrogen peroxide (30&amp;nbsp;wt%)</td><td>Fisher</td><td>H325</td><td>Certified ACS</td></tr><tr><td>10-ml syringes</td><td>Fisher</td><td>14-823-16E</td><td></td></tr><tr><td>Dual channel syringe pump</td><td>Cole Parmer</td><td>EW-74900-10</td><td>Or equivalent programmable dual channel syringe pump</td></tr><tr><td>Tygon tubing 1/8 inch ID, 1/4 inch OD</td><td>Cole Parmer</td><td>EW-0640776</td><td></td></tr><tr><td>Tygon tubing 1/16 inch ID, 1/8 inch OD</td><td>Cole Parmer</td><td>EW-0740771</td><td></td></tr><tr><td>0.1-&amp;micro;m Nylon filter</td><td>Fisher</td><td>R01SP04700</td><td></td></tr><tr><td>Labquake shaker rotisserie</td><td>Thermo Scientific</td><td>4002110Q</td><td></td></tr></tbody></table>

synthesis and reaction chemistry of nanosize monosodium titanate

Dieses Papier beschreibt die Synthese und Peroxid-Modifizierung von nanoskaligem Mononatrium Titanat (nMST), zusammen mit einer Ionenaustauschreaktion des Materials mit Au (III) -Ionen zu beladen. Das Syntheseverfahren wurde aus einem Sol-Gel-Verfahren abgeleiteten verwendet Mikrometergrße Mononatrium Titanat (MST), mit mehreren wichtigen Modifikationen erzeugen, einschließlich Reagenzkonzentrationen Verändern einer Partikel seed Schritt weggelassen, und ein nicht-ionisches Tensid Einführung Kontrolle zu erleichtern Partikelbildung und Wachstum. Das resultierende Material zeigt nMST kugelförmige Partikelmorphologie mit einer monodispersen Verteilung der Teilchendurchmesser in dem Bereich von 100 bis 150 nm. Die nMST Material gefunden wurde -1 eine Brunauer-Emmett-Teller (BET) -Oberfläche von 285 m 2 g zu haben, die höher ist als die mikrometergroßen MST mehr als eine Größenordnung ist. Der isoelektrische Punkt des nMST gemessen 3,34 pH-Einheiten, die eine pH-Einheit niedriger als die für den Mikrometergröße MST gemessen wird. Ter nMST Material gefunden wurde, als eine wirksame Ionenaustauscher unter schwach zur Herstellung von Au (III) -Austausch nanotitanate sauren Bedingungen zu dienen. Zusätzlich wurde die Bildung des entsprechenden peroxotitanate durch Reaktion des nMST mit Wasserstoffperoxid nachgewiesen.

MST synthetisiert wird ein Sol-Gel-Verfahren verwendet, bei dem Tetraisopropoxytitan (IV) (TIPT), Natriummethoxid und Wasser kombiniert und umgesetzt in Isopropanol Keimteilchen von MST zu bilden. 4 Micron großen Teilchen werden dann durch kontrollierte Zugabe von zusätzlichen gewachsen Mengen der Reagenzien. Die resultierenden Teilchen sind mit einem amorphen Kern und eine äußere Faserbereich Abmessungen von etwa 10 nm breiten Länge von 50 nm. 20 1A zeigt ...

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Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

Synthese und Reaktionschemie von nanoskaligen Mononatrium Titanat

This paper describes the synthesis and peroxide-modification of nanosize monosodium titanate (nMST), along with an ion-exchange reaction to load the ...

synthesis-and-reaction-chemistry-of-nanosize-monosodium-titanate

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Chemical Equilibria

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8.6K Aufrufe.  Savannah River Consulting, L.L.C.. The surfactant mediated sol-gel synthesis of nanosized monosodium titanate is described, along with preparation of the corresponding peroxide modified material. An ion-exchange reaction with Au(III) is also presented.

Serie: Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate

Preparation of Silica Nanoparticles Through Microwave-assisted Acid-catalysis

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle diameters ranging from 30-250 nm by varying the reaction conditions. Through the selection of a microwave compatible solvent, silicic acid precursor, catalyst, and microwave irradiation time, these microwave-assisted methods were capable of overcoming the previously reported shortcomings associated with synthesis of silica nanoparticles using microwave reactors. The siloxane precursor was hydrolyzed using the acid catalyst, HCl. Acetone, a low-tan &#948; solvent, mediates the condensation reactions and has minimal interaction with the electromagnetic field. Condensation reactions begin when the silicic acid precursor couples with the microwave radiation, leading to silica nanoparticle sol formation. The silica nanoparticles were characterized by dynamic light scattering data and scanning electron microscopy, which show the materials&#39; morphology and size to be dependent on the reaction conditions. Microwave-assisted reactions produce silica nanoparticles with roughened textured surfaces that are atypical for silica sols produced by St&#246;ber&#39;s methods, which have smooth surfaces.

Silica nanoparticles were prepared using acid-catalysis of a siloxane precursor and microwave-assisted synthetic techniques resulting in the controlled growth of nanomaterials ranging from 30-250 nm in diameter. The growth dynamics can be controlled by varying the initial silicic acid concentration, time of the reaction, and temperature of reaction.

Herstellung von Silica-Nanopartikeln durch Mikrowellen-unterstützte Säure-Katalyse

Microwave-assisted synthetic techniques were used to quickly and reproducibly produce silica nanoparticle sols using an acid catalyst with nanoparticle ...

Forschung

Chemie

Fabrication of Spatially Confined Complex Oxides

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from the inherent strong electron correlations that reside within them. These materials can also possess electronic phase separation in which regions of vastly different resistive and magnetic behavior can coexist within a single crystal alloy material. By reducing the scale of these materials to length scales at and below the inherent size of the electronic domains, novel behaviors can be exposed. Because of this and the fact that spin-charge-lattice-orbital order parameters each involve correlation lengths, spatially reducing these materials for transport measurements is a critical step in understanding the fundamental physics that drives complex behaviors. These materials also offer great potential to become the next generation of electronic devices 1-3. Thus, the fabrication of low dimensional nano- or micro-structures is extremely important to achieve new functionality. This involves multiple controllable processes from high quality thin film growth to accurate electronic property characterization. Here, we present fabrication protocols of high quality microstructures for complex oxide manganite devices. Detailed descriptions and required equipment of thin film growth, photo-lithography, and wire-bonding are presented.

We describe the use of pulsed laser deposition (PLD), photolithography and wire-bonding techniques to create micrometer scale complex oxides devices. The PLD is utilized to grow epitaxial thin films. Photolithography and wire-bonding techniques are introduced to create practical devices for measurement purposes.

Herstellung von räumlich getrennter komplexe Oxide

Complex materials such as high Tc superconductors, multiferroics, and colossal magnetoresistors have electronic and magnetic properties that arise from ...

Ingenieurwesen

Atomically Defined Templates for Epitaxial Growth of Complex Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain such surfaces are described. The first approach is the preparation of single terminated perovskite SrTiO3 (001) and DyScO3 (110) substrates. Wet etching was used to selectively remove one of the two possible surface terminations, while an annealing step was used to increase the smoothness of the surface. The resulting single terminated surfaces allow for the heteroepitaxial growth of perovskite oxide thin films with high crystalline quality and well-defined interfaces between substrate and film. In the second approach, seed layers for epitaxial film growth on arbitrary substrates were created by Langmuir-Blodgett (LB) deposition of nanosheets. As model system Ca2Nb3O10- nanosheets were used, prepared by delamination of their layered parent compound HCa2Nb3O10. A key advantage of creating seed layers with nanosheets is that relatively expensive and size-limited single crystalline substrates can be replaced by virtually any substrate material.

Various procedures are outlined to prepare atomically defined templates for epitaxial growth of complex oxide thin films. Chemical treatments of single crystalline SrTiO3 (001) and DyScO3 (110) substrates were performed to obtain atomically smooth, single terminated surfaces. Ca2 Nb3 O10- nanosheets were used to create atomically defined templates on arbitrary substrates.

Atomar definierte Vorlagen Epitaxieausrüstung komplexer Oxide Thin Films

Atomically defined substrate surfaces are prerequisite for the epitaxial growth of complex oxide thin films. In this protocol, two approaches to obtain ...

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and reduction half reactions, and fast electron (hole) diffusion and charge separation. Nanowires present suitable architectures to meet these requirements. Axially segmented Ag|ZnO and radially segmented (coaxial) TiO2-Ag nanowires with a diameter of 200 nm and a length of 6-20 &#181;m were made by templated electrodeposition within the pores of polycarbonate track-etched (PCTE) or anodized aluminum oxide (AAO) membranes, respectively. In the photocatalytic experiments, the ZnO and TiO2 phases acted as photoanodes, and Ag as cathode. No external circuit is needed to connect both electrodes, which is a key advantage over conventional photo-electrochemical cells. For making segmented Ag|ZnO nanowires, the Ag salt electrolyte was replaced after formation of the Ag segment to form a ZnO segment attached to the Ag segment. For making coaxial TiO2-Ag nanowires, a TiO2 gel was first formed by the electrochemically induced sol-gel method. Drying and thermal annealing of the as-formed TiO2 gel resulted in the formation of crystalline TiO2 nanotubes. A subsequent Ag electrodeposition step inside the TiO2 nanotubes resulted in formation of coaxial TiO2-Ag nanowires. Due to the combination of an n-type semiconductor (ZnO or TiO2) and a metal (Ag) within the same nanowire, a Schottky barrier was created at the interface between the phases. To demonstrate the photocatalytic activity of these nanowires, the Ag|ZnO nanowires were used in a photocatalytic experiment in which H2 gas was detected upon UV illumination of the nanowires dispersed in a methanol/water mixture. After 17 min&#160;of illumination, approximately 0.2 vol% H2 gas was detected from a suspension of ~0.1 g of Ag|ZnO nanowires in a 50 ml 80 vol% aqueous methanol solution.

Preparation and Use of Photocatalytically Active Segmented Ag|ZnO and Coaxial TiO2-Ag Nanowires Made by Templated Electrodeposition

Procedures are outlined to prepare segmented and coaxial nanowires via templated electrodeposition in nanopores. As examples, segmented nanowires consisting of Ag and ZnO segments, and coaxial nanowires consisting of a TiO2 shell and a Ag core were made. The nanowires were used in photocatalytic hydrogen formation experiments.

Herstellung und Verwendung von photokatalytisch aktiven segmentierte Ag | ZnO und TiO Koaxial<sub&gt; 2</sub&gt; Ag-Nanodrähte Hergestellt von gestützte Elektrochemische Abscheidung

Photocatalytically active nanostructures require a large specific surface area with the presence of many catalytically active sites for the oxidation and ...

Reverse Microemulsion-mediated Synthesis of Monometallic and Bimetallic Early Transition Metal Carbide and Nitride Nanoparticles

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The silica-encapsulated metal oxide nanoparticles are then carburized in a methane/hydrogen atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal carbide nanoparticles. During the carburization process, the silica shells prevent the sintering of adjacent carbide nanoparticles while also preventing the deposition of excess surface carbon. Alternatively, the silica-encapsulated metal oxide nanoparticles can be nitridized in an ammonia atmosphere at temperatures over 800 &#176;C to form silica-encapsulated early transition metal nitride nanoparticles. By adjusting the reverse microemulsion parameters, the thickness of the silica shells, and the carburization/nitridation conditions, the transition metal carbide or nitride nanoparticles can be tuned to various sizes, compositions, and crystal phases. After carburization or nitridation, the silica shells are then removed using either a room-temperature aqueous ammonium bifluoride solution or a 0.1 to 0.5 M NaOH solution at 40-60 &#176;C. While the silica shells are dissolving, a high surface area support, such as carbon black, can be added to these solutions to obtain supported early transition metal carbide or nitride nanoparticles. If no high surface area support is added, then the nanoparticles can be stored as a nanodispersion or centrifuged to obtain a nanopowder.

A &#8220;removable ceramic coating method&#8221; is presented in visual format for the synthesis of non-sintered and metal-terminated monometallic and bimetallic early transition metal carbide and nitride nanoparticles with tunable sizes and crystal structures.

Umkehrmikroemulsion-vermittelte Synthese von Monometallische und Bimetall frühes Übergangsmetall Carbide und Nitride Nanopartikel

A reverse microemulsion is used to encapsulate monometallic or bimetallic early transition metal oxide nanoparticles in microporous silica shells. The ...

Synthesis and Characterization of Fe-doped Aluminosilicate Nanotubes with Enhanced Electron Conductive Properties

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe aims at lowering the band gap of imogolite, an insulator with the chemical formula (OH)3Al2O3SiOH, and at modifying its adsorption properties towards azo-dyes, an important class of organic pollutants of both wastewater and groundwater.
Fe-doped nanotubes are obtained in two ways: by direct synthesis, where FeCl3 is added to an aqueous mixture of the Si and Al precursors, and by post-synthesis loading, where preformed nanotubes are put in contact with a FeCl3&#8226;6H2O aqueous solution. In both synthesis methods, isomorphic substitution of Al3+ by Fe3+ occurs, preserving the nanotube structure. Isomorphic substitution is indeed limited to a mass fraction of ~1.0% Fe, since at a higher Fe content (i.e., a mass fraction of 1.4% Fe), Fe2O3 clusters form, especially when the loading procedure is adopted. The physicochemical properties of the materials are studied by means of X-ray powder diffraction (XRD), N2 sorption isotherms at -196 &#176;C, high resolution transmission electron microscopy (HRTEM), diffuse reflectance (DR) UV-Vis spectroscopy, and &#950;-potential measurements. The most relevant result is the possibility to replace Al3+ ions (located on the outer surface of the nanotubes) by post-synthesis loading on preformed imogolite without perturbing the delicate hydrolysis equilibria occurring during nanotube formation. During the loading procedure, an anionic exchange occurs, where Al3+ ions on the outer surface of the nanotubes are replaced by Fe3+ ions. In Fe-doped aluminosilicate nanotubes, isomorphic substitution of Al3+ by Fe3+ is found to affect the band gap of doped imogolite. Nonetheless, Fe3+ sites on the outer surface of nanotubes are able to coordinate organic moieties, like the azo-dye Acid Orange 7, through a ligand-displacement mechanism occurring in an aqueous solution.

Here, we present a protocol to synthesize and characterize Fe-doped aluminosilicate nanotubes. The materials are obtained by either sol-gel synthesis upon addition of FeCl3&#8226;6H2O to the mixture containing the Si and Al precursors or by post-synthesis ionic exchange of preformed aluminosilicate nanotubes.

Synthese und Charakterisierung von Fe-dotierten Aluminosilikatgerüststoffe Nanoröhrchen mit Enhanced Electron leitenden Eigenschaften

The goal of the protocol is to synthesize Fe-doped aluminosilicate nanotubes of the imogolite type with the formula (OH)3Al2-xFexO3SiOH. Doping with Fe ...

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs within the interlayer space of semiconducting layered titania nanosheet (TNS) films was investigated here. Two types of intermediate films (i.e., TNS films containing methyl viologen (TNS/MV2+) and 2-ammoniumethanethiol (TNS/2-AET+)) were prepared. The two intermediate films were soaked in an aqueous tetrachloroauric(III) acid (HAuCl4) solution, whereby considerable amounts of Au(III) species were accommodated within the interlayer spaces of the TNS films. The two types of obtained films were then soaked in an aqueous sodium tetrahydroborate (NaBH4) solution, whereupon the color of the films immediately changed from colorless to purple, suggesting the formation of AuNPs within the TNS interlayer. When only TNS/MV2+ was used as the intermediate film, the color of the film gradually changed from metallic purple to dusty purple within 30 min, suggesting that aggregation of AuNPs had occurred. In contrast, this color change was suppressed by using the TNS/2-AET+ intermediate film, and the AuNPs were stabilized for over 4 months, as evidenced by the characteristic extinction (absorption and scattering) band from the AuNPs.

In Situ Synthesis of Gold Nanoparticles without Aggregation in the Interlayer Space of Layered Titanate Transparent Films

Here, we present a protocol for the in situ synthesis of gold nanoparticles (AuNPs) within the interlayer space of layered titanate films without the aggregation of AuNPs. No spectral change was observed even after 4 months. The synthesized material has expected applications in catalysis, photo-catalysis, and the development of cost-effective plasmonic devices.

In - situ - Synthese von Gold - Nanopartikeln ohne Aggregation zwischen die Schichten von Layered - Titanat OHP - Folien

Combinations of metal oxide semiconductors and gold nanoparticles (AuNPs) have been investigated as new types of materials. The in situ synthesis of AuNPs ...

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical photocatalytic structures. However, the influence of such chemical bonding on the optical and surface properties of the photocatalyst and thus its photocatalytic activity/reaction selectivity behavior has not been systematically studied. In this investigation, TiO2 has been supported on the surface of SiO2 by means of two different methods: (i) by the in situ formation of TiO2 in the presence of sand quartz via a sol-gel method employing tetrabutyl orthotitanium (TBOT); and (ii) by binding the commercial TiO2 powder to quartz on a surface silica gel layer formed from the reaction of quartz with tetraethylorthosilicate (TEOS). For comparison, TiO2 nanoparticles were also deposited on the surfaces of a more reactive SiO2 prepared by a hydrolysis-controlled sol-gel technique as well as through a sol-gel route from TiO2 and SiO2 precursors. The combination of TiO2 and SiO2, through interfacial Ti-O-Si bonds, was confirmed by FTIR spectroscopy and the photocatalytic activities of the obtained composites were tested for photocatalytic degradation of NO according to the ISO standard method (ISO 22197&#8722;1). The electron microscope images of the obtained materials showed that variable photocatalyst coverage of the support surface can successfully be achieved but the photocatalytic activity towards NO removal was found to be affected by the preparation method and the nitrate selectivity is adversely affected by Ti-O-Si bonding.

The Effect of Interfacial Chemical Bonding in TiO2-SiO2 Composites on Their Photocatalytic NOx Abatement Performance

The focus of the present work is to establish means to generate and quantify levels of Ti-O-Si linkages and to correlate these with the photocatalytic properties of the supported TiO2.

Die Wirkung der interfacialen chemischen Bindung in TiO<sub&gt; 2</sub&gt; -SiO<sub&gt; 2</sub&gt; Verbundwerkstoffe über ihre photokatalytische NOx-Abfallleistung

The chemical bonding of particulate photocatalysts to supporting material surfaces is of great importance in engineering more efficient and practical ...

Chemical Synthesis of Porous Barium Titanate Thin Film and Thermal Stabilization of Ferroelectric Phase by Porosity-Induced Strain

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its well-balanced ferroelectricity, piezoelectricity, and dielectric constant. In addition, BT does not contain any toxic elements. Therefore, it is considered to be an eco-friendly material, which has attracted considerable interest as a replacement for lead zirconate titanate (PZT). However, bulk BT loses its ferroelectricity at approximately 130 &#176;C, thus, it cannot be used at high temperatures. Because of the growing demand for high-temperature ferroelectric materials, it is important to enhance the thermal stability of ferroelectricity in BT. In previous studies, strain originating from the lattice mismatch at hetero-interfaces has been used. However, the sample preparation in this approach requires complicated and expensive physical processes, which are undesirable for practical applications.
In this study, we propose a chemical synthesis of a porous material as an alternative means of introducing strain. We synthesized a porous BT thin film using a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles were used as an organic template. Through a series of studies, we clarified that the introduction of pores had a similar effect on distorting the BT crystal lattice, to that of a hetero-interface, leading to the enhancement and stabilization of ferroelectricity. Owing to its simplicity and cost effectiveness, this fabrication process has considerable advantages over conventional methods.

Here, we present a protocol for the synthesis of porous barium titanate (BaTiO3) thin film by a surfactant-assisted sol-gel method, in which self-assembled amphipathic surfactant micelles are used as an organic template.

Chemische Synthese von porösen Barium-Titanat Dünnschicht und thermische Stabilisierung der ferroelektrischen Phase von Porosität-induzierten Belastung

Barium titanate (BaTiO3, hereafter BT) is an established ferroelectric material first discovered in the 1940s and still widely used because of its ...

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of Manganese(II) Acetylacetonate

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in magnetic resonance imaging (MRI). While iron oxide nanoparticles provide constant negative contrast on MRI over typical experimental timeframes, MnO generates switchable positive contrast on MRI through dissolution of MnO to Mn2+ at low pH within cell endosomes to &#8216;turn ON&#8217; MRI contrast. This protocol describes a one-pot synthesis of MnO nanoparticles formed by thermal decomposition of manganese(II) acetylacetonate in oleylamine and dibenzyl ether. Although running the synthesis of MnO nanoparticles is simple, the initial experimental setup can be difficult to reproduce if detailed instructions are not provided. Thus, the glassware and tubing assembly is first thoroughly described to allow other investigators to easily reproduce the setup. The synthesis method incorporates a temperature controller to achieve automated and precise manipulation of the desired temperature profile, which will impact resulting nanoparticle size and chemistry. The thermal decomposition protocol can be readily adapted to generate other metal oxide nanoparticles (e.g., iron oxide) and to include alternative organic solvents and stabilizers (e.g., oleic acid). In addition, the ratio of organic solvent to stabilizer can be changed to further impact nanoparticle properties, which is shown herein. Synthesized MnO nanoparticles are characterized for morphology, size, bulk composition, and surface composition through transmission electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy, respectively. The MnO nanoparticles synthesized by this method will be hydrophobic and must be further manipulated through ligand exchange, polymeric encapsulation, or lipid capping to incorporate hydrophilic groups for interaction with biological fluids and tissues.

Manganese Oxide Nanoparticle Synthesis by Thermal Decomposition of ManganeseII Acetylacetonate

This protocol details a facile, one-pot synthesis of manganese oxide (MnO) nanoparticles by thermal decomposition of manganese(II) acetylacetonate in the presence of oleylamine and dibenzyl ether. MnO nanoparticles have been utilized in diverse applications including magnetic resonance imaging, biosensing, catalysis, batteries, and waste water treatment.

Manganoxid-Nanopartikelsynthese durch thermische Zersetzung von Mangan(II) Acetylacetonat

For biomedical applications, metal oxide nanoparticles such as iron oxide and manganese oxide (MnO), have been used as biosensors and contrast agents in ...

Synthese und Reaktionschemie von nanoskaligen Mononatrium Titanat

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