Name: synthesis and reaction chemistry of nanosize monosodium titanate
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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.

Nano monosodyum Titanate 1. N- (Nmst) <ol><li> titanyum izopropoksit 1.8 ml, ardından izopropanol 7.62 ml ağırlıkça% 25 sodyum metoksit çözeltisi 0.58 ml ekleyerek çözeltisi 1. 10 ml hazırlayın. </li><li> izopropanol 9.76 ml ultra saf su 0.24 ml ekleyerek çözüm # 2 10 ml hazırlayın. </li><li> (: 625 g / mol, ortalama molekül ağırlığı), Triton X-100, 0.44 ml, ardından, bir 3 boyunlu 500 ml&#39;lik yuvarlak tabanlı bir şişeye izopropanol 280 ml ilave edilir. Manyetik bir karıştırma çubuğuna sahip olan iyi bir çözelti ilave edin. </li><li> 0.333 ml / dakika bir oranda çözüm # 1 ve # 2 sunmak için bir çift kanal şırınga pompası hazırlayın. </li><li> Yük çözeltiler 500 ml&#39;lik yuvarlak tabanlı bir şişe içinde çözelti seviyesinin altında şırıngayla çözeltinin teslim sağlayacak bir boru uzunluğunu ile donatılmış iki ayrı 10 ml&#39;lik şırınga # 1 ve # 2. </li><li> Karıştırılırken, 1.4 adım programlanmış şırınga pompası kullanılarak reaksiyona çözeltiler # 1 ve # 2 (her biri 10 mL) her ekleyin. </li> &lt;İlave işlemi tamamlandıktan sonra, li&gt; balon kap ve oda sıcaklığında 24 saat boyunca karıştırılmaya devam etmektedir. </li><li> şişeyi kapağını açmak ve reaksiyon karışımı ısı ~ 45-90 dakika boyunca 82 ° C&#39;de (geri akan izopropanol), ısıtma muhafaza edilirken, nitrojen ile temizlenerek ve ardından yine. izopropanol buharlaştırılır olarak buharlaştırılarak izopropanol yerine aralıklı olarak ultra saf su ekleyin. </li><li> izopropanol en buharlaştırıldı ve eklenen suyun hacmi, yaklaşık 50 ml sonra, ısıyı uzaklaştırmak ve reaksiyon karışımı soğumaya bırakın. </li><li> 0.1-um naylon filtre kağıdından filtre ürünü toplamak ve yüzey aktif madde ve herhangi bir artık izopropanol çıkarmak için su ile bir kaç kez yıkayın. kuruyana kadar filtre yok. Yıkama işlemi tamamlandıktan sonra, önceden tartılmış bir şişe veya bir şişe içine filtre çamuru transferi ve sulu bir bulamaç halinde saklayın. </li><li> bulamacın katı ağırlık yüzdelerine belirlenerek verimi belirlemek. Bunun bir eş payı ağırlığı ölçülerek yapılabilirönce ve kurutulduktan sonra bulamaç. </li></ol> 2. Au (III) İyon Değişimi <ol><li> 50 ml bir santrifüj tüpüne 4.23 ağırlıkça% Nmst bulamacın 6.50 g aktarın. Bu miktar, yukarıda adım 1.10 üretilen Nmst bulamacın gerçek ağırlık yüzdesine dayanıldığında, ve adım 1.11 belirlenen değişebilir. </li><li> 1-dram cam şişenin içine HAuCl 4 · 3H 2 O 0,0659 g tartılır. Hedef Ti: Au kütle oranı 4: 1. </li><li> Su ~ 1 ml HAuCl 4 · 3H H2O içinde çözülür, daha sonra Nmst ihtiva eden bir santrifüj tüpüne aktarılır. 2 O Nmst ihtiva eden bir santrifüj tüpüne aktarılır HAuCl 4 · 3H tüm sağlamak için ek su ile şişe birkaç kere yıkayın. </li><li> 11 ml toplam hacmi getirmek için, gerektiğinde ek su ile süspansiyon seyreltilir. yaklaşık 15 mM arasındaki nihai bir Au (III) &#39;ün konsantrasyonu hedef. </li><li> Karanlıkta süspansiyon tutmak için folyo ile santrifüj tüp sarın birdaha sonra 4 gün, en az bir çalkalama rotisserie ilgili süspansiyon çamaşır d. </li><li> 15 dk katı izole etmek için 3000 xg santrifüj ürünü toplayın. 15 dakika bir değişime uğramamış Au (III) &#39;kaldırmak için 3000 x g&#39;de santrifüj ile suda yeniden dağıtılmasıyla, katılar damıtılmış su ile üç kere yıkanır ve reizolatı. </li><li> Her iki suda yeniden dağıtılmasıyla bir sulu süspansiyon halinde, ya da nihai yıkama suyu boşaltılarak ve tüp sınırı ile nemli bir katı olarak nihai ürün saklayın. Karanlıkta ürünü saklayın. </li></ol> Peroxotitanate 3. hazırlanması <ol><li> Küçük bir şişeye Nmst bir 9.8 ağırlık% bulamacın 5 g aktarın. </li><li> Ağırlıkça% 30 H2O 2 çözeltisi 0.154 g tartılır. Hedef H2O 2: Ti molar oranı 0.25: 1 &#39;dir. </li><li> Nmst süspansiyon karıştırılırken de 2 O 2 çözeltisi damla damla H 0.154 g ekleyin. WHI H2O 2 Ekleme üzerine, süspansiyon,te katılar hemen sarıya döner. </li><li> İlave işlemi tamamlandıktan sonra, 24 saat süre ile, oda sıcaklığında reaksiyon karıştırıldı. </li><li> 0.1-um naylon filtre vasıtasıyla filtre ürünü toplamak ve reaksiyona girmemiş H 2 O 2 çıkarmak için su ile bir kaç kez yıkayın. kuruyana kadar filtre yok. Yıkama işlemi tamamlandıktan sonra, önceden tartılmış bir şişe veya bir şişe içine filtre çamuru transferi ve sulu bir bulamaç halinde saklayın. </li></ol>

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The authors have nothing to disclose.

gereksiz Suyun varlığı, saf olmayan reaktifler, örneğin, reaksiyon sonucu değiştirebilir daha büyük ya da daha fazla çok yönlü dağılmış parçacıkların yol açar. Bu nedenle, bakım kuru reaktifler kullanılmasını sağlamak için önlemler alınmalıdır. Titanyum izopropoksit ve sodyum metoksit kullanılmadığı zaman bir kurutucuda saklanmalıdır. Yüksek saflıkta izopropanol, aynı zamanda sentez için kullanılmalıdır. Sıcaklık formu parçacık bir jel ürünü ...

Titan dioksit ve alkali metal titanatlar yaygın olarak boya ve cilt bakım ürünleri pigment olarak ve enerji dönüşümü ve kullanımında fotokatalizörlerin olarak çeşitli uygulamalar kullanılmaktadır. 1-3 sodyum titanatlar katyonların bir dizi kaldırma etkili malzemeler olduğu gösterilmiştir katyon değiştirme reaksiyonları ile pH koşullarının geniş bir aralıkta. 4-7 Yukarıda açıklanan uygulamalara ek olarak, mikron büyüklüğünde sodyum titanatlar ve sodyum peroxotitanates en son da terapötik metal elde etme platformu olarak gösterilmiştir. Bu uygulamada, örneğin Au (III) &#39;ün, Au (I)&#39; in, Pt (II) olarak terapötik metal iyonları monosodyum titanat sodyum iyonları (MST) için değiştirilir. In vitro testler asal metal değişimli titanatlar olan bastırılmasını göstermektedir bilinmeyen bir mekanizma ile kanser ve bakteriyel hücrelerin büyümesi. 8,9 Tarihsel olarak, sodyum titanatlar olmak varen sol-jel ve bir kaç birkaç yüz mikron arasında değişen ebatlarda ince tozlar elde hidrotermal sentez teknikleri kullanarak üretilen. 4,5,10,11 Daha yakın zamanda, sentetik metotlar nanoboyutlu titanyum dioksit üretilen bildirilmiştir, metal- katkılı titanyum oksitler, ve diğer metal titanatlar çeşitli. Örnekler, sodyum, titanyum oksit nanotüpler (NaTONT) ya da nanotelleri, yüksek sıcaklık ve basınçta, fazla sodyum hidroksit içinde titanyum dioksit reaksiyonu ile, yüksek sıcaklık ve basınçta, 15 ve sodyum de aşırı sodyum hidroksid ile peroksotitanik asitin reaksiyonu sureti ile 12-14 sodyum titanat nanolifler içerir ve asit ile-yer değiştirilmiş mikron boyutunda titanatlann delaminasyonu ile nanolifler sezyum titanat. 16 nanoboyutlu sodyum titanatlar ve sodyum peroxotitanates sentezi genellikle filmin difüzyon veya intraparticle DIFFU tarafından kontrol edilen iyon değişim kinetiğinin, geliştirmek için ilgi çekicidirsion. Bu mekanizmalar, büyük ölçüde, iyon değiştirici parçacık boyutu ile kontrol edilir. Buna ek olarak, tedavi edici bir metal taşıyıcı platformu olarak, titanat malzemenin parçacık boyutu önemli ölçüde metal alışverişinde titanat ve kanser ve bakteri hücreleri arasındaki etkileşimin doğasını etkileyecek beklenir. Örneğin, 0.5 mertebesinde tipik olarak bakteri hücreleri, - 2 um, nano boyutlu parçacıkların karşı mikron boyutlu parçacıklar farklı etkileşimler olasılıkla olurdu. Buna ek olarak, fagositik olmayan ökaryotik hücreler sadece, böylece en az 1 mikron. 17 partikül büyüklüğü içselleştirme gösterilmiştir, nanoboyutlu sodyum titanatlar sentezi de titanat dağıtım platformdan metal elde etme ve hücresel alımını kolaylaştırmak için ilgi çekmektedir. Sodyum titanatlar ve peroxotitanates boyutunu küçültme da metal iyonu ayrımları etkili kapasitesini artırmak ve malzemenin fotokimyasal özelliklerini artıracaktır. 16,18 &lt;/ sup&gt; Bu makale hafif sol-jel koşullarında nanoboyutlu monosodyum titanat (Nmst) sentezlemek için geliştirilen bir protokol tanımlamaktadır 19 Nmst modifiye ilgili peroksit hazırlanmasını.; Au ile Nmst (III) yüklemek için bir iyon değişim reaksiyonu ile de tarif edilmektedir.

<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

Bu çalışma, Au (III) iyonları ile malzemenin yüklenmesi, bir iyon-değişim reaksiyonu ile, sentez ve nanoboyutlu monosodyum titanat peroksit modifikasyonu (Nmst) tarif etmektedir. Sentez yöntemi, reaktif konsantrasyonunu değiştiren bir partikül tohumu aşamasının atlanması ve kontrolünü kolaylaştırmak için iyonik olmayan bir yüzey aktif madde sokulması dahil olmak üzere çeşitli önemli değişiklikler ile mikron büyüklüğünde monosodyum titanat (MST) üretilmesi için kullanılan bir sol-jel işlemi türetildi partikül oluşumu ve büyümesi. Elde edilen Nmst malzemesi 100 ile 150 nm aralığı içinde parçacık çaplarının bir tek dağılımlı dağılımı olan küresel şekilli parçacık morfolojisi sergiler. Nmst malzemesi mikron boyutunda MST daha yüksek bir büyüklük sırasına göre daha 285 m2 g-1, bir Brunauer-Emmett-Teller (BET) bir yüzey alanına sahip olduğu bulunmuştur. Nmst izoelektrik noktası mikron boyut MST için ölçülen daha pH birimi daha düşüktür 3.34 pH birimi, ölçülen. TO malzeme Au (III) &#39;ün-değişimi nanotitanate hazırlanması için zayıf asidik koşullar altında etkili bir iyon değiştiricisi olarak görev bulunmuştur Nmst. Buna ek olarak, karşılık gelen peroxotitanate oluşumu hidrojen peroksit ile Nmst reaksiyonu ile gösterilmiştir.

MST tetraizopropoksititanyum (IV) &#39;ün (TIPT), sodyum metoksit ve su birleştirildiği bir sol-jel yöntemi ile sentezlenmiş ve MST tohum parçacıklarının oluşturulması için, izopropanol içinde reaksiyona sokulur. 4 mikron-boyutlu parçacıkları, daha sonra ilave kontrollü eklenmesiyle büyütülür reaktifler miktarları. Elde edilen parçacıklar amorf çekirdek ve uzunluğu 50 nm çapında yaklaşık 10 nm boyuta sahip bir dış elyaflı bölge bulunur. 20 <p class="jove_conten...

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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.

Nanoboyutlu Monosodyum Titanate Sentezi ve Reaksiyon Kimya

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

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8.6K Görüntüleme.  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.

Video: 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.

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

Kimya

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.

Mekansal Kapalı Karmaşık Oksitler Fabrikasyon

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

Mühendislik

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.

Karmaşık Oksit İnce Filmlerin Epitaksiyel Büyüme için atomik Tanımlı Şablonlar

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.

Hazırlık ve foto Aktif Bölümlü Ag Kullanım | ZnO ve Koaksiyel TiO<sub&gt; 2</subTemplated elektrodepozisyon tarafından yapılmıştır&gt;-Ag Nanoteller

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.

Monometalik ve Bimetalik Erken Geçiş Metal Carbide ve Nitrür Nanopartiküller Ters Mikroemülsiyon aracılı sentezi

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.

Geliştirilmiş Elektron İletken özellikleri ile Fe-katkılı Alüminosilikat Nanotüpler Sentezi ve Karakterizasyonu

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.

Katmanlı Titanate Şeffaf Filmleri Interlayers Uzayda Toplama olmadan Altın Nanopartiküller Yerinde Sentez

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.

Yüzeyel Kimyasal Yapıştırmanın TiO&#39;ya Etkisi<sub&gt; 2</sub&gt; -SiO<sub&gt; 2</sub&gt; Fotokatalitik NOx Azaltma Performansına Sahip Kompozitler

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.

Kimyasal sentez gözenekli baryum Titanate ince Film ve Ferroelectric faz porozite indüklenen gerilim tarafından termal stabilizasyon

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.

Manganez(II) Asetofonat Termal Ayrıştırma ile Manganez Oksit Nanopartikül Sentezi

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

Nanoboyutlu Monosodyum Titanate Sentezi ve Reaksiyon Kimya

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