Name: synthesis and reaction chemistry of nanosize monosodium titanate
Uploaded: 2016-02-23T14:00:00.000+00:00
Duration: 8 min 44 s
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.

ナノモノナトリウムチタン酸の1の合成（nMST） <ol><li>チタンイソプロポキシドの1.8ミリリットル、続いてイソプロパノール7.62ミリリットル〜25重量％ナトリウムメトキシド溶液の0.58ミリリットルを添加することにより、溶液＃1の10ミリリットルを準備します。 </li><li>イソプロパノールの9.76ミリリットルに超純水の0.24ミリリットルを添加することにより、溶液＃2の10ミリリットルを準備します。 </li><li>トリトンX-100（：625グラム/モルの平均MW）の0.44ミリリットル、続いて三首500mlの丸底フラスコにイソプロパノールの280ミリリットルを追加します。磁気攪拌棒をうまく解決策をかき混ぜます。 </li><li> 0.333ミリリットル/分の速度でソリューション＃1と＃2を提供するデュアルチャネルシリンジポンプを準備します。 </li><li>ロードソリューション500mlの丸底フラスコ内の溶液レベル以下にシリンジポンプからの溶液の配信を可能にするチューブの長さを装備二つの別々の10-mlの注射器への＃1、＃2。 </li><li>撹拌しながら、ステップ1.4でプログラムシリンジポンプを用いて反応するソリューション＃1、＃2（各10ml）のすべてを追加します。 </li> &lt;添加が完了した後李&gt;は、フラスコに蓋をし、室温で24時間撹拌し続けます。 </li><li>フラスコにキャップを取ると、45〜90分間の〜82℃（還流イソプロパノール）反応混合物を加熱し、加熱を維持しながら、窒素でパージしました。イソプロパノールが蒸発するように、蒸発させてイソプロパノールを置換するために断続的に超純水を加えます。 </li><li>イソプロパノールのほとんどを蒸発させ、水の添加量が約50 mlであるした後、熱を除去し、反応混合物を冷却することを可能にします。 </li><li> 0.1μmのナイロンフィルター紙を通して濾過することにより生成物を収集し、界面活性剤及び残留イソプロパノールを取り除くために水で数回洗浄します。乾燥するまでフィルタリングしないでください。洗浄が完了した後、予め秤量した瓶またはバイアルにフィルターからスラリーを転送し、水性スラリーとして保存します。 </li><li>スラリーの重量％の固形分を決定することによって、収量を決定します。これのアリコートの重量を測定することによって行うことができます乾燥前と後のスラリー。 </li></ol> 2.金（III）イオン交換<ol><li> 50-ml遠心チューブに4.23重量％nMSTスラリーの6.50グラムを転送します。この金額は、上記のステップ1.10で生産nMSTスラリーの実際の重量パーセントに基づいて、ステップ1.11で決定して変化し得ます。 </li><li> 1ドラムのガラスバイアルにのHAuCl 4・3H 2 Oの0.0659グラムを量り分けます。ターゲットTiが1：Auの質量比は4です。 </li><li>水〜1ミリリットル中のHAuCl 4・3H 2 Oを溶解し、その後nMSTを含む遠心管に移します。 3H 2 O・のHAuCl 4の全てを確実にするために、追加の水でバイアルを数回すすぎnMSTを含む遠心管に移します。 </li><li> 11ミリリットルに全量を、必要に応じて、追加の水で懸濁液を希釈します。約15mmの最後の金（III）濃度をターゲットにしています。 </li><li> 、暗闇の中での懸濁液を保つためにホイルで遠心分離管を包みますその後、最低4日間シェーカーロティサリーにサスペンションをタンブルdは。 </li><li>固形物を分離するために15分間、3000×gで遠心分離することによって、製品を収集します。任意の未交換のAu（III）を除去するために15分間、3000×gで遠心分離することにより、水に再分散することにより、蒸留水で固形分を3回洗浄し、そしてreisolate。 </li><li>いずれかの水に再分散することにより水性懸濁液として、または最終洗浄水をデカントし、チューブをキャッピングすることにより湿った固形物として最終製品を保管してください。暗所で保管してください。 </li></ol> Peroxotitanateの調製<ol><li>小さなフラスコにnMSTの9.8重量％スラリーの5グラムを転送します。 </li><li> 30重量％H 2 O 2溶液 0.154グラム量り分けます。目標H 2 O 2：Tiのモル比は0.25：1です。 </li><li> nMST懸濁液を攪拌しながらも、H 2 O 2溶液の滴下の0.154グラムを追加します。 WHIのH 2 O 2添加すると、サスペンションteの固体がすぐに黄色に変わります。 </li><li>添加が完了した後、24時間周囲温度で反応を撹拌しました。 </li><li> 0.1μmのナイロンフィルターを通して濾過することにより生成物を収集し、未反応のH 2 O 2を除去するために水で数回洗浄します。乾燥するまでフィルタリングしないでください。洗浄が完了した後、予め秤量した瓶またはバイアルにフィルターからスラリーを転送し、水性スラリーとして保存します。 </li></ol>

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The authors have nothing to disclose.

余分な水の存在は、不純な試薬から、例えば、より大きなまたはより多分散の粒子をもたらす、反応の結果を変えることができます。そのため、注意が乾燥反応物が使用されているように注意しなければなりません。チタンイソプロポキシドおよびナトリウムメトキシドは、使用しないときはデシケーター中に保存しなければなりません。高純度イソプロパノールも合成のために使用される?...

二酸化チタンとアルカリ金属チタン酸塩は、広くそのような塗料やスキンケア製品における顔料として、エネルギー変換および利用における光触媒として様々な用途に使用されている。1-3ナトリウムチタネートは、陽イオンの範囲を除去するのに有効な材料であることが示されています陽イオン交換反応によってpH条件の広い範囲にわたって4-7 今述べた用途に加えて、ミクロンサイズのナトリウム、チタン酸ナトリウムperoxotitanates最近、治療金属配信プラットフォームとして機能することが示されています。このアプリケーションでは、例えばAu（III）などの治療用金属イオンは、金（I）、およびPt（II）は、一ナトリウムチタネート（MST）のナトリウムイオンと交換される。貴金属交換チタン酸塩を用いたin vitro試験での抑制を示します未知のメカニズムによる癌および細菌細胞の増殖。8,9 歴史的には、ナトリウムチタネートがあることしていますENは、ゾル-ゲル及び少数から数百ミクロンの範囲の粒子サイズを有する微粉末が得られ、水熱合成技術の両方を使用して製造。4,5,10,11より最近では、合成方法は、ナノサイズの二酸化チタンを生じたことが報告されている、金属-ドープ酸化チタン、および他の金属チタン酸塩の様々な。例としては、ナトリウム、酸化チタンナノチューブ（NaTONT）またはナノワイヤ高温高圧で過剰の水酸化ナトリウム中の二酸化チタンの反応によって、高められた温度および圧力、15ナトリウムで過剰の水酸化ナトリウムを有するペルオキソチタン酸の反応により12-14チタン酸ナトリウムナノファイバーを含みます酸交換ミクロンサイズのチタン酸塩の層間剥離することによりナノファイバーチタン酸セシウム。16 ナノサイズのナトリウム、チタン酸ナトリウムperoxotitanatesの合成は、典型的には、フィルムの拡散または粒子内diffuによって制御され、イオン交換速度を高めるために重要ですシオン。これらのメカニズムは、主にイオン交換体の粒径によって制御されます。また、治療用金属配信プラットフォームとして、チタン材の粒径が大きく、金属交換チタン酸癌と細菌細胞との間の相互作用の性質に影響を与えると予想されます。例えば、0.5のオーダーで、典型的には、細菌細胞、 - 2μmでは、ナノサイズ粒子対ミクロンサイズの粒子と異なる相互作用を可能性を有するであろう。また、非食真核細胞は、1ミクロン未満のサイズの粒子を内部にのみ示されている。17このように、ナノサイズのナトリウムチタン酸塩の合成は、チタン酸配信プラットフォームからの金属の送達および細胞取り込みを容易にするために、関心もあります。ナトリウムチタネート及びperoxotitanatesのサイズを小さくすると、金属イオンの分離において有効容量を増加させ、材料の光化学的特性を強化する。16,18 &lt;/ SUP&gt;本稿では、軽度のゾル-ゲル条件下でナノサイズのモノナトリウム、チタン酸（nMST）を合成するために開発したプロトコルを記述し19 nMST修正、対応する過酸化物の製造を。金とnMST（III）をロードするためのイオン交換反応と一緒にも記載されています。

<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

本論文では、Au（III）イオンを有する材料をロードするためにイオン交換反応とともに、合成とナノサイズのモノナトリウム、チタン酸の過酸化修飾（nMST）について説明します。合成法は、粒子種ステップを省略し、試薬濃度を変化させることを含むいくつかの主要な修飾で、ミクロンサイズのモノナトリウムチタネート（MST）を生成するために使用されるゾル - ゲルプロセスから誘導される、との制御を容易にするために、非イオン性界面活性剤を導入しました。粒子形成と成長。得nMST材料は、100〜150 nmの範囲の粒径の単分散分布を有する球状の粒子形態を示します。 nMST材料はミクロンサイズMSTよりも高い桁以上で285 m 2とgで-1のブルナウアー-エメット-テラー（BET）表面積を有することが見出されました。 nMSTの等電点は、ミクロンサイズMSTについて測定よりも低いpH単位で3.34のpH単位を測定しました。 T彼は材料が金（III）-exchangeのナノチタンの製造のための弱酸性条件下での効果的なイオン交換体として機能することがわかったnMST。また、対応するperoxotitanateの形成は、過酸化水素とnMSTの反応によって実証されました。

MSTは、テトライソプロポキシチタン（IV）（TIPT）、ナトリウムメトキシド、および水を合わせ、MSTのシード粒子を形成するために、イソプロパノール中で反応させる。4ミクロンサイズの粒子は、追加の制御された添加によって成長させられたゾル-ゲル法を用いて合成されます試薬の量。得られた粒子は、長さが50ナノメートルによって幅約10nmの寸法を有するアモルファスコアと外?...

Watch this Scientific Journal Video about Synthesis and Reaction Chemistry of Nanosize Monosodium Titanate at JoVE.com

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.

ナノサイズ一ナトリウムチタン酸の合成と反応化学

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 ビュー.  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.

ビデオ: 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.

マイクロ波支援酸 - 触媒反応によりシリカナノ粒子の調製

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

化学

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.

空間的に閉じ込められた複合酸化物の作製

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

工学

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.

複合酸化物薄膜のエピタキシャル成長のために原子的に定義されたテンプレート

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.

ZnOと同軸のTiO |光触媒活性セグメント化銀の調製および使用<sub&gt; 2</subテンプレート化電製&gt; - 銀ナノワイヤー

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.

モノとバイメタル早期遷移金属炭化物と窒化物ナノ粒子の逆マイクロエマルジョン媒介合成

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.

強化された電子導電特性を持つFeドープアルミノシリケートナノチューブの合成とキャラクタリゼーション

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.

層状チタン酸透明フィルムの層間空間で凝集することなく金ナノ粒子のその場合成で

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.

TiOにおける界面化学結合の影響<sub&gt; 2</sub&gt; -SiO<sub&gt; 2</sub&gt;光触媒NOx低減性能に関する複合材料

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.

化学合成チタン酸バリウム多孔質セラミックス薄膜の気孔率誘起歪による強誘電相の熱安定化

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.

マンガンの熱分解による酸化マンガンナノ粒子合成(II) アセチルアセトネート

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

ナノサイズ一ナトリウムチタン酸の合成と反応化学

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